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United States Patent |
5,296,050
|
Takamiya
,   et al.
|
March 22, 1994
|
Method of producing grain oriented silicon steel sheets having improved
magnetic properties
Abstract
This invention not only improves the formation of fine crystal structure
and hence the magnetic properties as well as surface properties while
utilizing the merits of the hot strip mill at maximum by conducting the
rough rolling in the steps for the production of grain oriented silicon
steel sheets, particularly hot rolling step at a high temperature and a
large draft, but also stably achieves the more improvement of the magnetic
properties under a high reliability by accurately controlling the
precipitation state of inhibitor at a finish rolling stage in the hot
rolling step.
Inventors:
|
Takamiya; Toshito (Chiba, JP);
Manabe; Masahiko (Chiba, JP);
Takeuchi; Fumihiko (Chiba, JP);
Obara; Takashi (Chiba, JP);
Iida; Yoshiaki (Kobe, JP)
|
Assignee:
|
Kawasaki Steel Corporation (JP)
|
Appl. No.:
|
925310 |
Filed:
|
August 4, 1992 |
PCT Filed:
|
May 8, 1990
|
PCT NO:
|
PCT/JP90/00586
|
371 Date:
|
January 7, 1991
|
102(e) Date:
|
January 7, 1991
|
PCT PUB.NO.:
|
WO90/13673 |
PCT PUB. Date:
|
November 15, 1990 |
Foreign Application Priority Data
| May 08, 1989[JP] | 1-113643 |
| May 16, 1989[JP] | 1-120337 |
| Oct 02, 1989[JP] | 1-255260 |
Current U.S. Class: |
148/111; 148/112; 148/504 |
Intern'l Class: |
C21D 009/46 |
Field of Search: |
148/110,111,112,504
|
References Cited
U.S. Patent Documents
4204891 | May., 1980 | Shiozaki et al. | 148/111.
|
4302257 | Nov., 1981 | Matsumoto et al. | 148/111.
|
4437909 | Mar., 1984 | Mori et al. | 148/111.
|
4473416 | Sep., 1984 | Kawamo et al. | 148/111.
|
5039359 | Aug., 1991 | Yoshitomi et al. | 148/111.
|
Foreign Patent Documents |
0118326 | Sep., 1979 | JP.
| |
61-12822 | Jan., 1986 | JP.
| |
1084327 | Apr., 1986 | JP.
| |
Primary Examiner: Dean; R.
Assistant Examiner: Ip; Sikyin
Attorney, Agent or Firm: Miller; Austin R.
Parent Case Text
This application is a continuation of application Ser. No. 07/634,202,
filed Jan. 7, 1991, now abandoned.
Claims
We claim:
1. A method of producing a grain oriented silicon steel sheet having
improved magnetic properties wherein a slab of silicon-containing steel,
after heating, is subjected to hot rolling comprising the steps of: rough
rolling at a temperature within a region exceeding 1150.degree. C. and
subsequent finish rolling said steel sheet, subjecting said steel sheet to
heavy cold rolling or cold rolling two times through intermediate
annealing to a final sheet thickness, subjecting said steel sheet to
decarburization annealing, applying a slurry of an annealing separator to
a surface of said steel sheet, and subjecting said steel sheet to final
finish annealing, characterized in that after said rough rolling occurs
within a temperature region exceeding 1150.degree. C., said finish rolling
is carried out at the temperature of the steel sheet is within a range of
1000.degree.-850.degree. C. at a percent reduction of not less than 40%
for 2-20% seconds to precipitate inhibitors in the steel sheet.
2. A method of producing a grain oriented silicon steel sheet having
improved magnetic properties wherein a slab of silicon-containing steel,
after heating, is subjected to hot rolling comprising the steps of: rough
rolling and subsequent finish rolling said steel sheet, subjecting said
steel sheet to heavy cold rolling or cold rolling two times through
intermediate annealing to a final sheet thickness, subjecting said steel
sheet to decarburization annealing, applying a slurry of an annealing
separator to a surface of said steel sheet, and subjecting said steel
sheet to final finish annealing, characterized in that in the finish hot
rolling step, said steel sheet is cooled while holding the temperature in
a central portion of said steel sheet in the thickness direction at a
value above 1150.degree. C., and when the sheet temperature positioned
from the surface at a depth corresponding to 1/20 of the sheet thickness
reaches a temperature in the range of 1000.degree.-950.degree. C., the
steel sheet is rolled at a present reduction of not less than 40% and held
at said temperature range for 3-20 seconds and then cooled, and when a
temperature at the central portion of said sheet reaches a central
temperature range of 950.degree.-850.degree. C., the steel sheet is rolled
at a percent reduction of not less than 40% and held at said central
temperature range for 2-20 seconds to precipitate uniformly and finely
dispersed inhibitor in the steel sheet.
3. A method of producing a grain oriented silicon steel sheet having
improved magnetic properties wherein a slab of silicon-containing steel,
after heating, is subjected to hot rolling comprising the steps of rough
rolling and subsequent finish rolling said steel sheet, subjecting said
steel sheet to a heavy cold rolling or a two-times cold rolling through an
intermediate annealing to a final sheet thickness, subjecting said steel
sheet to decarburization annealing, applying a slurry of an annealing
separator to a surface of said steel sheet, and subjecting said steel
sheet to a final finish annealing, characterized in that at said rough
rolling step, a first pass is carried out under conditions that a rolling
temperature T.sub.1 is not lower than 1280.degree. C. and percent
reduction R.sub.1 satisfies the following equation:
60.gtoreq.R.sub.1 (%).gtoreq.-0.5T.sub.1 +670
and wherein said steel sheet is held under the above conditions up to a
next pass for not less than 30 seconds, and a final pass is carried out
under conditions that a rolling temperature R.sub.2 is not lower than
1200.degree. C. and percent reduction R.sub.2 satisfies the following
equation:
70.gtoreq.R.sub.2 (%).gtoreq.-0.3T.sub.2 +165.
4. A method of producing a grain oriented silicon steel sheet having
improved magnetic properties wherein a slab of silicon-containing steel,
after heating, is subjected to hot rolling comprising the steps of rough
rolling and subsequent finish rolling said steel sheet, subjecting said
steel sheet to a heavy cold rolling or a two-times cold rolling through an
intermediate annealing to a final sheet thickness, subjecting said steel
sheet to decarburization annealing, applying a slurry of an annealing
separator to a surface of said steel sheet, and subjecting said steel
sheet to a final finish annealing, characterized in that at said rough
rolling step, a first pass is carried out under conditions that a rolling
temperature T.sub.1 is not lower than 1280.degree. C. and percent
reduction R.sub.1 satisfies the following equation:
60.gtoreq.R.sub.1 (%).gtoreq.-0.5T.sub.1 +670
and wherein said steel sheet is held under the above conditions up to a
next pass for not less than 30 seconds, and a final pass is carried out
under conditions that a rolling temperature T.sub.2 is not lower than
1200.degree. C. and percent reduction R.sub.2 satisfies the following
equation:
70.gtoreq.R.sub.2 (%).gtoreq.-0.3T.sub.2 +165
and then finish rolling is carried out within a temperature range of
1000.degree.-850.degree. C. at a percent reduction of not less than 40%
and held at said temperature range for 2-20 seconds.
5. A method of producing a grain oriented silicon steel having improved
magnetic properties wherein a slab of silicon-containing steel, after
heating, is subjected to hot rolling comprising the steps of rough rolling
and subsequent finish rolling said steel sheet, subjecting said steel
sheet to a heavy cold rolling or a two-times cold rolling through an
intermediate annealing to a final sheet thickness, subjecting said steel
sheet to decarburization annealing, applying a slurry of an annealing
separator to a surface of said steel sheet, and subjecting said steel
sheet to a final finish annealing, characterized in that at said rough
rolling step, a first pass is carried out under conditions that a rolling
temperature T.sub.1 is not lower than 1280.degree. C. and percent
reduction R.sub.1 satisfies the following equation:
60.gtoreq.R.sub.1 (%).gtoreq.-0.5T.sub.1 +670
and wherein said steel sheet is held under the above conditions up to a
next pass for not less than 30 seconds, and a final pass is carried out
under conditions that a rolling temperature T.sub.2 is not lower than
1200.degree. C. and percent reduction R.sub.2 satisfies the following
equation:
70.gtoreq.R.sub.2 (%).gtoreq.-0.3T.sub.2 +165
and at said subsequent finish rolling stage, said steel sheet is cooled
while holding the temperature in a central portion of said steel sheet in
the thickness direction above 1150.degree. C., and when the temperature at
a depth corresponding to 1/20 of the sheet thickness reaches a temperature
range of 1000.degree.-950.degree. C., the steel sheet is rolled at a
percent reduction of not less than 40% and held at the above temperature
range for 3-20 seconds and then cooled, and when the temperature at the
central portion reaches a temperature range of 950.degree.-850.degree. C.,
the steel sheet is rolled at a present reduction of not less than 40% and
held at said temperature range for 2-20 seconds.
6. A method of producing a grain oriented silicon steel sheet in any of
claims 1, 2, 3, 4 or 5, wherein the temperatures of heating said slab is
not lower than 1370.degree. C. in a central portion of said slab.
7. A method of producing a grain oriented silicon steel sheet having
improved magnetic properties wherein a slab of silicon-containing steel,
after heating, is subjected to hot rolling comprising the steps of: rough
rolling at a temperature within a region exceeding 1150.degree. C.,
subsequent finish rolling said steel sheet and precipitating uniformly and
finely dispersed inhibitor in said steel sheet, subjecting said steel
sheet to heavy cold rolling or cold rolling two times through intermediate
annealing to a final sheet thickness, subjecting said steel sheet to
decarburization annealing applying a slurry of an annealing separator to a
surface of said steel sheet, and subjecting said steel sheet to final
finish annealing, characterized in that after said rough rolling occurs
within a temperature region exceeding 1150.degree. C., said finish rolling
is carried out within a temperature range of 1000.degree.-850.degree. C.
at a percent reduction of not less than 40% for 2-20 seconds.
Description
TECHNICAL FIELD
This invention relates to a method of producing grain oriented silicon
steel sheets having improved magnetic properties.
1. Background of the Invention
As is well-known, grain oriented silicon steel sheets are mainly used as a
material for iron core in transformers and other electrical machinery and
equipment and are comprised of secondary recrystallized grains aligned
{110} face to plate face and <001> axis to rolling direction. In order to
develop the secondary recrystallized grains having such a crystal
orientation, it is required that precipitates such as MnS, MnSe, AlN and
the like called as an inhibitor are uniformly and finely dispersed in
steel to effectively suppress growth of crystal grains in an orientation
other than {110}<001> orientation during the final annealing at a high
temperature. Therefore, the control of the inhibitor dispersed state is
carried out by solid-soluting these precipitates in the slab heating prior
to hot rolling at once and then subjecting to a hot rolling having a
proper cooling pattern.
Here, an important role of the hot rolling lies in that the solid-soluted
inhibitor components are finely and uniformly precipitated as an
inhibitor.
2. Description of the Prior Art
For example, Japanese Patent laid open No. 53-39852 has reported that a
proper dispersion phase of MnSe is obtained by holding the steel sheet
within a temperature range of not lower than 850.degree. C. but not higher
than 1200.degree. C. for 60-360 seconds. In this method, however, the
inhibitor is ununiform and coarsely precipitated in a fair frequency.
Particularly, it is experientially known that the inhibitor becomes
considerably coarse when being held at about 1100.degree. C. for a long
period of time. Therefore, this method is difficult to provide a complete
secondary recrystallized structure because the inhibiting force of the
inhibitor decreases.
Furthermore, Japanese Patent Application Publication No. 58-13606 has
proposed a method wherein the steel sheet is cooled at a cooling rate of
not less than 3.degree. C./s while being continuously subjected to a hot
rolling within a temperature range of 950.degree.-1200.degree. C. at a
draft of not less than 10%. In this method, however, the inhibitor is not
always finely precipitated, and the coarse or nonuniform precipitation of
the inhibitor is caused in accordance with the size of crystal grains.
Particularly, the dispersion in a direction of sheet thickness is apt to
become nonuniform. As a cause, there is mentioned a nonuniformity of
strain inherent to high temperature deformation.
In these conventional methods, the dispersed state of the inhibitor can not
completely be rendered into a fine and uniform state, and the normal
growth of primary crystal grains can not effectively be controlled at a
secondary recrystallization annealing step in final finish annealing, so
that the complete secondary recrystallization structure can not be
obtained.
Another important role of the hot rolling lies in that the slab cast
structure is made fine by recrystallization to form a structure most
suitable for secondary recrystallization. Moreover, such a treatment for
increasing the fineness of the crystal structure has hitherto been carried
out apart from the solid solution treatment of the inhibitor.
As to the solid solution of the inhibitor, it has hitherto been reported,
for example, in Japanese Patent laid open No. 63-10911 that grain oriented
silicon steel sheets having less surface defect and good properties are
obtained by raising the slab surface temperature above 1320.degree. C. to
a temperature of 1420.degree.-1495.degree. C. at a temperature rising rate
of not less than 8.degree. C./min when holding the slab surface
temperature within a range of 1420.degree.-1495.degree. C. for 5-60
minutes. According to this method, the complete solid solution of the
inhibitor has certainly be achieved and also the coarsening of the slab
surface grains can be suppressed in principle to improve the surface
properties, but it is actually difficult to uniformly satisfy the above
condition against a heavy article such as a slab or the like, and
particularly it is impossible in fact to completely suppress the
coarsening of crystal grains over the full length of the slab. Therefore,
in order to ensure the uniformity of the structure, it is required to add
any treatment for finely dividing the crystal grains during the hot
rolling.
On the other hand, as to the formation of fine structure, there are known
many methods, i.e. a method of rolling under a high draft through
recrystallization within a temperature range of 1190.degree.-960.degree.
C. (Japanese Patent laid open No. 54-120214), a method of rolling under a
high draft of not less than 30% at a state containing not less than 3% of
.gamma.-phase within a temperature range of 1230.degree.-960.degree. C.
(Japanese Patent laid open No. 55-119216), a method of restricting a
starting temperature for rough rolling to not higher than 1250.degree. C.
(Japanese Patent laid open No. 57-11614), a method of rolling at a strain
rate of not more than 15 s.sup.-1 and a draft of not less than 15%/one
pass within a temperature range of 1050.degree.-1200.degree. C. (Japanese
Patent laid open No. 59-93828), and the like. These methods are common in
a point that the formation of fine structure is carried out by rolling
under a high draft at a temperature region of about 1200.degree. C. That
is, they are based on recrystallization limits reported in
"Tetsu-to-Hagane", 67 (1981) S 1200 or is based on the same technical idea
as described above. FIG. 4 shows this knowledge. From this figure, it is
understood that the rolling at high temperature does not substantially
contribute to the recrystallization and only the application of large
strain at a low temperature recrystallization region contributes to the
recrystallization. Therefore, it is necessary to conduct the rolling after
the cooling to not higher than 1250.degree. C. in order to form the fine
structure through the recrystallization even in the slab heated to high
temperature.
In all of the above techniques, the heating temperature is not lower than
1250.degree. C., and the upper limit thereof is not particularly
restricted, so that it is common in a point that the inhibitor is
solid-soluted by holding in a furnace for a long period of time while
allowing the grain growth of the slab to a certain extent and the crystal
grains are finely divided by hot rolling.
Considering the actual state of these method, however, when the slab is
heated at a high temperature for completely solid-soluting the inhibitor,
it is required to not only arrange a cooling means at an upstream side of
hot strip mill but also take an extra mill power for conducting the hot
rolling at a low temperature, which is conflicting with the idea of hot
strip mill aiming at the energy-saving and the high productivity.
Furthermore, the effect of the rolling at the low temperature is not
necessarily clear.
That is, when the above method is applied to actual steps, many problems
are existent though the effect, is developed to a certain extent.
OBJECTS OF THE INVENTION
A first object of the invention is to provide a method of advantageously
producing grain oriented silicon steel sheets, in which improved magnetic
properties are stably obtained by conducting sufficiently uniform and fine
dispersion of the inhibitor at the hot rolling step.
A second object of the invention is to provide a method of advantageously
producing grain oriented silicon steel sheets having improved magnetic
properties and further surface properties, in which a fine and uniform
crystal structure is reliably obtained while utilizing mass production as
a merit of hot strip mill at maximum even under a condition of
high-temperature slab heating useful for the complete solid-solution of
the inhibitor and the improvement of surface properties.
SUMMARY OF THE INVENTION
The feature and construction of the invention are as follows. 1. A first
embodiment includes a method of producing a grain oriented silicon steel
sheet having improved magnetic properties by a series of steps of
subjecting a slab of silicon-containing steel to hot rolling comprised of
rough rolling and subsequent finish rolling after heating, subjecting to a
heavy cold rolling or a two-times cold rolling through an intermediate
annealing to a final sheet thickness, subjecting to decarburization
annealing, applying a slurry of an annealing separator to a surface of a
steel sheet, and subjecting to a final finish annealing, characterized in
that at the above hot rolling step, said finish rolling is carried out at
a draft of not less than 40% within a temperature range of
1000.degree.-850.degree. C. followed to said rough rolling within a
temperature region exceeding 1150.degree. C., and the above temperature
range is held for 2-20 seconds. 2. A second embodiment includes a method
of producing a grain oriented silicon steel sheet having improved magnetic
properties by a series of steps of subjecting a slab of silicon-containing
steel to hot rolling comprised of rough rolling and subsequent finish
rolling after heating, subjecting to a heavy cold rolling or a two-times
cold rolling through an intermediate annealing to a final sheet thickness,
subjecting to decarburization annealing, applying a slurry of an annealing
separator to a surface of a steel sheet, and subjecting to a final finish
annealing, characterized in that at said finish rolling stage in the above
hot rolling step, said steel sheet is cooled while holding the temperature
in a central portion of said steel sheet in the thickness direction above
1150.degree. C., and when a temperature positioned from the surface into a
depth corresponding to 1/20 of the sheet thickness reaches to a
temperature range of 1000.degree.-950.degree. C., the steel sheet is
rolled at a draft of not less than 40% and held at the above temperature
range for 3-20 seconds and then cooled, and when a temperature at the
central portion reaches to a temperature range of 950.degree.-850.degree.
C., the steel sheet is rolled at a draft of not less than 40% and held at
this temperature range for 2-20 seconds. 3. A third embodiment includes a
method of producing a grain oriented silicon steel sheet having improved
magnetic properties by a series of steps of subjecting a slab of
silicon-containing steel to hot rolling comprised of rough rolling and
subsequent finish rolling after heating, subjecting to a heavy cold
rolling or a two-times cold rolling through an intermediate annealing to a
final sheet thickness, subjecting to decarburization annealing, applying a
slurry of an annealing separator to a surface of a steel sheet, and
subjecting to a final finish annealing, characterized in that at said
rough rolling stage in said hot rolling step, a first pass is carried out
under conditions that a rolling temperature T.sub.1 is not lower than
1280.degree. C. and a draft R.sub.1 satisfies the following equation:
60.gtoreq.R.sub.1 (%).gtoreq.0.5T.sub.1 +670
and held under the above conditions up to a next pass for not less than 30
seconds, and a final pass is carried out under conditions that a rolling
temperature T.sub.2 is not lower than 1200.degree. C. and a draft R.sub.2
satisfies the following equation:
70.gtoreq.R.sub.2 (%).gtoreq.0.1T.sub.2 +165
4. A fourth embodiment includes a method of producing a grain oriented
silicon steel sheet having improved magnetic properties by a series of
steps of subjecting a slab of silicon-containing steel to hot rolling
comprised of rough rolling and subsequent finish rolling after heating,
subjecting to a heavy cold rolling or a two-times cold rolling through an
intermediate annealing to a final sheet thickness, subjecting to
decarburization annealing, applying a slurry of an annealing separator to
a surface of a steel sheet, and subjecting to a final finish annealing,
characterized in that at said rough rolling stage in said hot rolling
step, a first pass is carried out under conditions that a rolling
temperature T.sub.1 is not lower than 1280.degree. C. and a draft R.sub.1
satisfies the following equation:
60.gtoreq.R.sub.1 (%).gtoreq.0.5T.sub.1 +670
and held under the above conditions up to a next pass for not less than 30
seconds, and a final pass is carried out under conditions that a rolling
temperature T.sub.2 is not lower than 1200.degree. C. and a draft R.sub.2
satisfies the following equation:
70.gtoreq.R.sub.2 (%).gtoreq.0.1T.sub.2 +165
and then said finish rolling is carried out within a temperature range of
1000.degree.-850.degree. C. at a draft of not less than 40% and held at
this temperature range for 2-20 seconds.
5. A fifth embodiment includes a method of producing a grain oriented
silicon steel sheet having improved magnetic properties by a series of
steps of subjecting a slab of silicon-containing steel to hot rolling
comprised of rough rolling and subsequent finish rolling after heating,
subjecting to a heavy cold rolling or a two-times cold rolling through an
intermediate annealing to a final sheet thickness, subjecting to
decarburization annealing, applying a slurry of an annealing separator to
a surface of a steel sheet, and subjecting to a final finish annealing,
characterized in that at said rough rolling stage in said hot rolling
step, a first pass is carried out under conditions that a rolling
temperature T.sub.1 is not lower than 1280.degree. C. and a draft R.sub.1
satisfies the following equation:
60-R.sub.1 (%).gtoreq.0.5T.sub.1 +670
and held under the above conditions up to a next pass for not less than 30
seconds, and a final pass is carried out under conditions that a rolling
temperature T.sub.2 is not lower than 1200.degree. C. and a draft R.sub.2
satisfies the following equation:
70.gtoreq.R.sub.2 (%).gtoreq.-0.1T.sub.2 165
and at said subsequent finish rolling stage, said steel sheet is cooled
while holding the temperature in a central portion of said steel sheet in
the thickness direction above 1150.degree. C., and when the temperature
positioned from the surface into a depth corresponding to 1/20 of the
sheet thickness reaches to a temperature range of 1000.degree.-950.degree.
C., the steel sheet is rolled at a draft of not less than 40% and held at
the above temperature range for 3-20 seconds and then cooled, and when a
temperature at the central portion reaches to a temperature range of
950.degree.-850.degree. C., the steel sheet is rolled at a draft of not
less than 40% and held at this temperature range for 2-20 seconds.
6. A sixth embodiment includes a method of producing a grain oriented
silicon steel sheet in the first, second, third, fourth and fifth
inventions, wherein a temperature of heating said slab is not lower than
1370.degree. C. as a temperature in a central portion of said slab.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagram showing influence of rolling temperature and holding
time on the precipitation state of an inhibitor;
FIG. 2 is a schematic view showing a preferable embodiment of heat
hysteresis for carrying out a second embodiment of the invention;
FIG. 3 is a graph showing a recystallization limit (recrystallinity of not
less than 95%) at single .alpha.-phase region by a relation between
rolling temperature and draft;
FIG. 4 is a graph showing a recrystallization limit at a (.alpha.+.beta.)
dual phase region;
FIG. 5 is a graph showing a recrystallization limit at a single
.alpha.-phase region after a first pass of the hot rough rolling;
FIG. 6 is a graph showing a relation between holding time and
recrystallinity after the rolling;
FIG. 7 is a graph showing a recrystallization limit at a single
.alpha.-phase region after plural passes of the hot rough rolling;
FIG. 8 is a graph showing changes of magnetic flux density in the
longitudinal direction of a steel sheet as a comparison between invention
examples and comparative examples;
FIG. 9 is a graph showing changes of magnetic flux density in the widthwise
direction of a steel sheet as a comparison between invention examples and
comparative examples; and
FIG. 10 is a graph showing a change of magnetic flux density in the
longitudinal direction of a steel sheet as a comparison among invention
examples and comparative examples.
DETAILED DESCRIPTION OF THE INVENTION
The invention will be described with respect to experimental results
succeeding in each of these inventions below.
At first, the experimental results on a uniform and fine dispersion of an
inhibitor will be described.
In general, when an element forming an inhibitor such as Se or the like is
precipitated and grown as MnSe or the like at a cooling stage after the
solid solution treatment, it has been proposed to control the size and
average interval of precipitated grains by the cooling rate, holding
temperature and holding time. However, the detail of precipitation
behavior required for the above control in the hot rolling is not
substantially clear up to the present, and particularly the relationship
between hot strain and precipitation of inhibitor is not clear, so that
the inhibitor could not uniformly and finely be precipitated over a full
surface of the steel sheet.
On the contrary, the inventors have made various studies with respect to
the precipitation behavior of the inhibitor at various temperature regions
and found out that the precipitation behavior of inhibitor largely changes
in accordance with the strain quantity applied at a high temperature and
the holding time of this temperature.
The inventors have made an experiment in a laboratory wherein Se was
completely solid-soluted by heating a steel slab and then strain was
applied at each temperature region and this temperature was held for a
given time. In this case, the strain quantity was varied by adopting a
draft of 0-70% and also the holding time was varied. From this experiment,
it was understood that the precipitation behavior of the inhibitor, in
which the precipitation rate was increased by applying strain, was
entirely different from a case of applying no strain. That is, the
experiment of applying no strain is unsuitable for investigating the
precipitation of inhibitor in the hot rolling. Furthermore, it has been
found that when the sheet was once cooled to room temperature at the
cooling stage before the precipitation treatment, the behavior was largely
different from that in the original cooling stage. Therefore, the
experiment was carried out by applying a proper hot working strain under
an accurate heat cycle.
An example of the experiments succeeding in the first embodiment of the
invention will be described below.
A slab of silicon steel comprising C: 0.045 wt% (hereinafter shown by %
simply), Si: 3.25%, Mn: 0.07%, Se: 0.020% and the reminder being
substantially Fe and having a thickness of 30 mm was subjected to a solid
solution treatment at 1350.degree. C. for 30 minutes and rapidly cooled to
a temperature giving a hot working strain, and then strain was applied by
rolling at a draft of 50% and held at the above temperature for varied
times.
In FIG. 1 is shown results examined on influences of each rolling
temperature exerting on the precipitation state of inhibitor and each
holding time at such a temperature.
Moreover, when the sheet is treated in the same cooling pattern without
applying strain, no precipitation of the inhibitor is caused until the
holding time is 60 seconds, so that the effect by the application of
strain is very large, and it has been confirmed that the introduction of
strain is indispensable for the precipitation of inhibitor in the hot
rolling.
From FIG. 1, it is clear that the nonuniform and coarse precipitation is
caused by applying strain at a temperature region exceeding 1000.degree.
C. However, no precipitation of inhibitor is caused when the temperature
exceeds 1150.degree. C.
On the contrary, the inhibitor is finely and uniformly precipitated at the
temperature region of 1000.degree.-850.degree. C., and in this case it has
been confirmed that the holding time of not less than 2 seconds is
required. However, when the holding time is too long, the precipitated
size of the inhibitor becomes larger, which produces the reduction of the
controlling force. Therefore, a holding time exceeding 20 seconds is not
favorable.
Furthermore, it has been found from FIG. 1 that the inhibitor is
nonuniformly and coarsely precipitated at high temperature, while the
inhibitor is uniformly and finely precipitated at low temperature side as
shown by the nonuniform precipitation region (1), coarse precipitation
region (2) and uniform and fine precipitation region (3).
As shown by a schematic view (1) of FIG. 1, the precipitation behavior at
high temperature is understood to center the precipitation onto
dislocations introduced by hot working strain and be influenced by the
dislocation density inside crystal. For this end, the inhibitor is apt to
precipitate on grain boundaries and subgrain boundaries, and the uniform
precipitation in the grains hardly occurs. On the contrary, the
precipitation behavior at low temperature as shown by a schematic view (3)
is caused irrespective of dislocations inside grain, so that the
precipitation becomes uniform inside the grains. The precipitation
behavior at low temperature is considered to be precipitation onto lattice
defects introduced by working strain, which is more uniform and finer than
the precipitation onto the dislocations observed at high temperature, so
that the inhibitor is uniformly and finely precipitated over a full
surface of the steel sheet. In this point, the feature that the
precipitation onto the dislocations becomes large at a high temperature is
considered due to the fact that the lattice defects introduced during
working rapidly dislocates and moves onto subgrain boundaries and grain
boundaries at the high temperature.
The quantity of hot working strain required is approximately a quantity
introduced by rolling at a cumulative draft of not less than 40% within
the above temperature range. This is because, the strain quantity
introduced into the crystal grains of the steel sheet actually differs in
every grain, so that the difference in the strain quantity between the
grains becomes large at a light draft and there is largely caused a fear
of differing the dispersion precipitation state of the inhibitor every
grain.
The following has been found from the above experimental results.
That is, when the hot strain is applied at a temperature region of
1000.degree.-850.degree. C., the precipitation nucleus of inhibitor is
formed at a very fast speed over the full surface inside the grain, and
also the precipitation is completed by holding at this temperature range
for 2-20 seconds, in which the dispersion state of the inhibitor in the
crystal grains becomes fine and uniform. That is, the completely fine and
uniform precipitation of the inhibitor is achieved over the full surface
of the steel sheet, and hence products having very excellent magnetic
properties are obtained.
The second embodiment of the invention will be described below.
Although the uniform and fine dispersion of the inhibitor is achieved by
the aforementioned treatment, when the surface state of the steel sheet
changes in accordance with the change of annealing temperature at
subsequent step of hot rolling, for example, at a primary
recrystallization annealing step, the inhibitor existing in the vicinity
of the surface is apt to become unstable. Therefore, in order to stably
produce the product having improved magnetic properties in industrial
scale, it has been found that it is required to minutely control the
dispersion precipitation state of the inhibitor in the direction of sheet
thickness.
The inventors have made studies on the results shown in FIG. 1 in detail
and found that slightly large inhibitor is obtained at the high
temperature even in the uniform precipitation region. That is, it has been
found that when strain is applied at a temperature region of
1000.degree.-950.degree. C. and this temperature region is held for not
less than 3 seconds, uniform but slightly large inhibitor is obtained.
This is considered due to the fact that even in the uniform precipitation
region, the high temperature side is less in the place forming nucleus for
the starting of precipitation and fast in the diffusion so that the
inhibitor somewhat grows as compared with the low temperature side.
Therefore, the size of the inhibitor can be controlled by utilizing the
above behavior.
As a result of examinations on the stabilization of inhibitor near to the
surface, it has been confirmed that when the size of the inhibitor near to
the surface is made somewhat large, the change of the inhibitor component
such as decomposition due to diffusion from the surface or the like at the
post step hardly occurs. Concretely, when the temperature of a layer
positioned from the surface to a depth corresponding to 1/20 of the sheet
thickness (hereinafter referred to as 1/20 layer) is within a range of
1000.degree.-950.degree. C., the best result is found to be obtained by
applying strain and then holding this temperature range for 3-20 seconds.
Thus, as the temperature at 1/20 layer and the precipitation state of
inhibitor near to the surface can be confirmed to be interrelated, it has
been clarified that the precipitation of the inhibitor near to the surface
can also be controlled by controlling the temperature at the 1/20 layer.
In brief, in order to finely and uniformly precipitate the inhibitor, the
application of working strain at the temperature region of
950.degree.-850.degree. C. is sufficient, while in order to uniformly
precipitate slightly large inhibitor, it is enough to apply the working
strain at the temperature region of 1000.degree.-950.degree. C.
Therefore, it is possible to separately control the dispersion state of the
inhibitor in the vicinity of the surface and the central portion by using
the above means, and the controlling force can stably be maintained in the
secondary recrystallization annealing without changing the surface
inhibitor in the primary recrystallization annealing and the
decarburization annealing.
In the actual hot rolling step, the slab is heated by gas and then the
temperature in the central portion of the slab is raised above
1370.degree. C. in an induction heating furnace to sufficiently ensure a
temperature difference to the surface and completely solid-solute the
inhibitor component, and thereafter the silicon steel sheet is cooled with
water at the sheet bar stage in the rough rolling to further adjust the
surface and central temperatures.
Then, when the temperature near to the surface or temperature located in
the layer corresponding to 1/20 of the sheet thickness is within a range
of 1000.degree.-950.degree. C. while holding the temperature in the
central portion of the sheet above 1150.degree. C. during the finish
rolling, the working strain is applied at a draft of not less than 40% and
subsequently the above temperature range is held for 3-20 seconds.
Further, when the temperature in the central portion is within a range of
950.degree.-850.degree. C. by cooling with water, the working strain is
applied at a draft of not less than 40% and the holding time at this
temperature range is held to 2-20 seconds to complete the hot finish
rolling.
FIG. 2 shows a preferable example of temperature hystresis in the finish
rolling. Moreover, the temperatures at the 1/20 layer and the central
layer were accurately simulated by means of a computer using finite
element method.
That is, when the temperature of the central portion is not lower than
1150.degree. C. and the temperature of the 1/20 layer is slightly lower
than 1000.degree. C., a first pass of the finish rolling is carried out to
ensure the holding time of at least 3 seconds until the temperature of the
1/20 layer is lower than 950.degree. C. Moreover, the rolling may further
be made during such a holding. Then, when the temperature of the central
portion is within a temperature range of 950.degree.-850.degree. C., the
rolling is carried out at a draft in total of not less than 40%. Moreover,
the rolling may be one pass or plural passes. In brief, the draft of not
less than 40% may be applied at each of the above temperature ranges.
According to the invention, it is important that the difference in the
temperature between the surface layer and the central portion just before
the finish rolling is sufficiently held. For this end, it is preferable to
sufficiently raise the temperature of the central portion by induction
heating. In order to ensure the difference in the temperature between the
central portion and the surface layer portion, it is favorable that the
surface layer portion is positively cooled with water at the sheet bar
stage.
The details elucidating the third embodiment of the invention will be
described below.
As previously mentioned, the achievement of formation of fine crystal
grains at higher temperature region is very useful for utilizing the mass
production as a merit of the hot strip mill.
Further, the inventors have made many experiments and studies on
recrystallization behavior at the high temperature region and newly found
that the recrystallization fully proceeds when the strain quantity is
sufficiently large even at the high temperature region which has hitherto
been considered as a strain recovering region and was not interest. In
this point, there is no report up to the present. Because, the high
temperature heating was difficult in industry, and even when being
examined in a laboratory, it was required to conduct the high temperature
heating for high temperature rolling, but there were caused problems such
as scale formation, repairing of experimental furnace and the like and
such a high temperature heating was very difficult.
Moreover, there are many experimental reports on ordinary steels. In this
case, the high temperature region above 1200.degree. C. is a dynamic
restoring region and is mainly restoring or dynamic recrystallization, so
that the examination exceeding these reports has not sufficiently been
made. Particularly, almost of the grain oriented silicon steels are
.alpha.-phase because they contain about 3% of Si. Since the .alpha.-phase
is considered to be easily restored, it seems that the dynamic
recrystallization does not occur in the grain oriented silicon steel,
which is entirely outside the interesting object.
However, the inventors have a question on such a common view and developed
a high temperature furnace capable of heating at a superhigh temperature
and having a less influence of scale and made various studies using such a
high temperature furnace, and as a result the aforementioned results have
been first accomplished.
The experiment succeeding in this invention will be described below.
A slab of silicon steel comprising C: 0.04%, Si: 3.36%, Mn: 0.05%, Se:
0.022% and the reminder being substantially Fe was heated at 1350.degree.
C. for 30 minutes, rolled at various temperatures under various drafts
through one pass and cooled with water, and thereafter the sectional
structure was observed to measure a recrystallinity.
The measured results are shown in FIG. 3 as a relation between rolling
temperature and draft.
As seen from this figure, it has been confirmed that the recrystallization
proceeds if the draft is not less than 30% even at a high temperature
region, for example, 1350.degree. C. which has been considered to generate
no recrystallization in the conventional knowledge. And also, it has been
found that the complete region of recrystallization is further enlarged by
holding the temperature for not less than 30 seconds, preferably not less
than 60 seconds after the rolling.
Such a phenomenon is understood as follows.
At first, it has been observed that subgrains constituted by rough
network-like dislocation structure are formed in unrecrystallized grains
after the rolling. Therefore, it is guessed that the restoring terminates
at a fairly fast time after the rolling. Furthermore, it is considered
that the roughness of the network or dislocation density is different in
the crystal grains so that such a difference of dislocation density is a
driving force of recrystallization. Since the grain boundary may be moved
by thermal activation at the high temperature, if the moved grain has a
curvature of not less than a certain value, it may be a nucleus for
recrystallization.
As a result of the above phenomenon, it has been clarified that the
recrystallization is actually possible even at the high temperature region
which has hitherto been considered to store not enough strain to cause the
dynamic recrystallization. Moreover, in this recrystallization behavior,
the dislocation density of the unrecrystallized region is low as mentioned
above, so that the driving force for the growth of the above region is
very small. However, when the mobility of the grain boundary is very large
or when the temperature is high (not lower than 1280.degree. C.), the
recrystallization is sufficiently possible though the time is required to
a certain extent.
This phenomenon is considerably different from the conventionally
well-known static recrystallization in the aspect.
The aforementioned fact is a case of rolling 3% silicon steel at a
temperature region above 1300.degree. C. or a recrystallization mechanism
at a single .alpha.-phase state, which is first revealed at this time. On
the contrary, the recrystallization limit curve conventionally well-known
in 3% silicon steel as shown in FIG. 4 is a case that hard .gamma.-phase
precipitates and the recrystallization is proceeded only in the vicinity
thereof. That is, the data are obtained by the rolling experiment in the
conventional technique, but the heat treating method prior to the rolling
is also omitted, so that it is considered that the results are different
from the experimental results making the basis of the invention. This is
considered due to the fact that the sample solid-soluted at a high
temperature was once cooled to room temperature and reheated to the given
rolling temperature for the rolling. In this case, .gamma.-phase is always
and partly produced in the structure. This .gamma.-phase is preferentially
produced near to the boundary of .alpha.-grains, at where the
recrystallization is easily proceeded. Even in this case, however, when
the original grain size is large as in the grains of the cast slab, the
recrystallization hardly completes, and the unrecrystallized portion is
always apt to be left in the central portion of the original grain.
Furthermore, the percentage and dispersion of .gamma.-phase are largely
dependent upon not only the temperature but also C, Si amounts as well as
strain quantity and cooling rate (holding time). Therefore, it is known
that the effect largely changes even in a slight change of the treating
condition. This is guessed to be a large reason why the effect of finely
dividing grains by low temperature hot rolling is not stably obtained in
the conventional technique. On the other hand, there is a drawback that
the increase of C amount (increase of coarse carbide) hardly provides the
rolling structure having a high alignment at post step.
On the contrary, the recrystallization behavior in single .alpha.-phase
region at high temperature found by the inventors is different from the
conventional recrystallization at low temperature in the presence of
.gamma.-phase, in which the forming site of recrystallization nucleus is
not .gamma.-phase but is merely the grain boundary. Furthermore, the size
of the recrystallized grain is apt to become relatively large, so that the
unrecrystallized portion hardly remains and the uniform recrystallized
grain structure is easily obtained.
Under the aforementioned recrystallization conditions at high temperature,
coarse grains can finely be divided even when the slab heated at high
temperature is rolled as it is. Furthermore, it is not required to render
the temperature into low temperature during the waiting for the rolling in
the course of the heating, so that the merit of the hot strip mill can be
utilized at maximum.
The third embodiment of the invention is accomplished based on the above
fundamental knowledges.
The construction of the third embodiment will be described in detail.
According to this invention, a slab of silicon steel having a chemical
composition as mentioned later is placed in a heating furnace and then
heated. Moreover, the heating temperature and heating time somewhat differ
in accordance with the kind and amount of the inhibitor, but it is
sufficient to ensure a time capable of achieving the complete solid
solution of the inhibitor. However, if the time existing in the furnace is
too long, a great amount of scale is created, so that the heating time is
rendered into an extent not to badly affect the surface properties. Thus,
the slab heated at the high temperature to render the inhibitor into a
complete solid solution state is subjected to a rough rolling.
The rough rolling is usually carried out at 5-6 passes. According to the
experimental results, it has been found that the first pass as well as the
subsequent holding and the final pass are particularly important. In the
holding after the first pass or just before the second pass, it is
important to obtain a substantially complete recrystallized structure
(recrystallinity: not less than 95%).
In FIG. 5 is shown a relation between the rolling temperature and the draft
exerting onto the recrystallization actually made in a factory.
In the usual rolling method, the time between the passes is determined by
the interval between stands of the rolling mill, in which the pass time
between first and second rough stands is about 20 seconds. Therefore, it
is very difficult to obtain a recrystallinity of not less than 95% just
after the rolling. As seen from FIG. 5, the recrystallinity of not less
than 95% can easily be obtained by holding the sheet for not less than 30
seconds, preferably not less than 60 seconds after the rolling.
In FIG. 6 is shown results measured on the proceeding state of
recrystallization when a first rolling pass is carried out at rolling
temperatures of 1280.degree. C. and 1300.degree. C. under a draft of 30%,
as a relation between the holding time after the rolling and the
recrystallinity.
As seen from FIG. 6, the higher the rolling temperature, the better the
recrystallization proceeding state, and when the rolling temperature is
1300.degree. C., the recrystallinity of 95% is attained for about 10
seconds. In this point, when the rolling temperature is as low as
1280.degree. C., about 30 seconds is required for obtaining
recrystallinity: 95%.
According to the invention, therefore, the rolling temperature in the first
pass of the rolling is determined to be not lower than 1280.degree. C.
When the relation between rolling temperature T.sub.1 .degree.C.) and draft
R.sub.1 (%) in the first pass capable of attaining the target
recrystallinity of 95% is calculated from the results of FIGS. 5 and 6,
the following equation is obtained:
60.gtoreq.R.sub.1 (%).gtoreq.-0.5T.sub.1 +670
In order to ensure the desired recrystallinity, it is required to hold the
sheet for not less than 30 seconds, preferably not less than 60 seconds
after the rolling.
And also, it has been found that the occurrence of spills resulting from
hot tears at the surface portion is fairly suppressed if the
recrystallization is completely attained at the first pass. Furthermore,
it has been found that the above condition effectively controls the
occurrence of the poor secondary recrystallized region through final
annealing due to the presence of the unrecrystallized portion.
In the rough rolling, it is important that the unrecrystallized portion is
not left in addition to the formation of fine recrystallization structure.
For this end, it is required to conduct the recrystallization at the
single .alpha.-phase region even in the final pass of the rough rolling.
Because, .gamma.-grains are harder in (.alpha.+.gamma.) dual phase region,
so that strain concentrates and is stored in the vicinity of
.gamma.-grains and such .gamma.-grains are preferentially recrystallized,
but .gamma.-grains mainly appear in old .alpha.-grains, and consequently
the structure always becomes nonuniform.
Since the crystal grains are finely recrystallized by the rolling effect
just before the final pass of the rough rolling, the recrystallization
limit shifts slightly downward from the experimental result in the factory
previously shown in FIG. 5 as shown in FIG. 7. Moreover, a region
appearing .gamma.-phase is shown in FIG. 7 by oblique lines, in which the
temperature appearing .gamma.-phase becomes high as the draft increases.
This is due to strain-induced transformation.
In the final pass, the rolling temperature T.sub.2 (.degree.C.) of at least
1200.degree. C. is required for conducting the rolling at the single
.alpha.-phase region not appearing .gamma.-phase. Furthermore, when a
relation between the rolling temperature T.sub.2 and draft R.sub.2 (%)
required for stably obtaining such a recrystallinity of not less than 75%
that the remaining unrecrystallized portion after the final pass does not
affect the degradation of secondary recrystallization at the final
annealing is calculated from the results of FIGS. 7 and 4, the following
equation was obtained:
70.gtoreq.R.sub.2 (%).gtoreq.-0.1T.sub.2 +165
Moreover, the upper limit of the draft in the rough rolling is necessary to
be set so as to ensure the sufficient draft even on the next pass and
after. From this viewpoint, the upper limits of the drafts in the first
pass and the final pass are limited to 60% and 70%, respectively.
The subsequent hot finish rolling may be conducted under conditions
according to the usual manner, but the more excellent effect is obtained
by combining the aforementioned first invention with the second invention.
Moreover, anyone of the conventionally well-known methods are applicable to
subsequent cold rolling, decarburization annealing, and final finish
annealing.
A preferable chemical composition of silicon-containing steel slab as a
starting material according to the invention will be described below.
C: 0.01-0.10%
C is an element useful for not only the formation of fine and uniform
structure in the hot rolling and the cold rolling but also the development
of Goss orientation. It is preferable to add carbon in an amount of at
least 0.01%. However, when the amount exceeds 0.10%, the disorder is
caused in the Goss orientation, so that the upper limit is preferably
about 0.10%.
Si: 2.0-4.5%
Si effectively contributes to enhance the specific resistance of the steel
sheet and reduce the iron loss thereof. When the amount exceeds 4.5%, the
cold ductility is damaged, while when it is less than 2.0%, not only the
specific resistance decreases, but also the randomization of crystal
orientation is caused due to .alpha.-.gamma. transformation during the
final high-temperature annealing required for secondary recrystallization
purification and the sufficiently iron loss-improving effect is not
obtained. Therefore, the Si amount is preferably about 2.0-4.5%.
Mn: 0.02-0.12%
Mn is required in an amount of at least about 0.02% for preventing the hot
tear, but when the amount is too large, the magnetic properties are
degraded, so that the upper limit is preferable to be defined to about
0.12%.
As the inhibitor, there are so-called MnS system, MnSe system and AlN
system.
Case of MnS, MnSe Systems
At least one one of Se and S: 0.005-0.06%
Each of Se, S is an element useful as an inhibitor controlling the
secondary recrystallization of the grain oriented silicon steel sheet.
From a viewpoint of ensuring the controlling force, an amount of at least
about 0.005% is required, but when it exceeds 0.06%, the effect is
damaged, so that the lower limit and upper limit are preferably about 0.01
and 0.06%, respectively.
Case of AlN System
Al: 0 005-0.10%, N: 0.004-0.015%
The ranges of Al and N are defined to the above ranges from the same reason
as in the aforementioned cases of MnS, MnSe systems. Moreover, the above
MnS, MnSe and AlN systems may be used together.
As the inhibitor component, Cu, Sn, Cr, Ge, Sb, Mo, Te, Bi and P are
advantageously adaptable in addition to the above S, Se, Al, so that they
may be included in small amounts together. The preferable addition ranges
of the above components are Cu, Sn, Cr: 0.01-0.15%, Ge, Sb, Mo, Te, Bi:
0.005-0.1%, P: 0.01-0.2%, and these inhibitor components may be used alone
or in admixture.
Moreover, the slab aiming to the invention is a continuously cast slab or a
slab obtained by blooming from an ingot, but naturally includes a slab
obtained by blooming and rerolling.
EXAMPLE 1
(A) Continuously cast slab comprising C: 0.040%, Si: 3.30%, Mn: 0.054%, Se:
0.022%, Sb: 0.024% and the remainder being substantially Fe.
(B) Continuously cast slab comprising C: 0.35%, Si: 2.98%, Mn: 0.072%, Se:
0.024%, Al: 0.023%, N: 0.008% and the remainder being substantially Fe.
Each of the above slabs (A) and (B) was placed in a heating furnace, soaked
in N.sub.2 atmosphere and subjected to rough rolling immediately after the
soaking. The rough rolling was carried out through 5-6 passes in
accordance with the slab thickness under such a condition that the draft
at each pass was approximately equal, whereby a sheet bar of 30 mm in
thickness was obtained. Then, the sheet bar was hot rolled in a tandem
mill to obtain a hot rolled steel sheet of 2.0 mm in thickness. The
temperature after the final pass of the rough rolling and conditions in
first pass of the finish rolling are shown in Table 1.
The hot rolled steel sheet was pickled, subjected to first cold rolling and
intermediate annealing and further to second cold rolling to obtain a cold
rolled steel sheet having a final thickness of 0.23 mm. Thereafter, the
cold rolled steel sheet was subjected to decarburization annealing, coated
with a slurry of an annealing separator consisting mainly of MgO, and then
subjected to a final finish annealing comprised of secondary
recrystallization annealing and purification annealing to obtain a
product.
The magnetic properties of the thus obtained product were measured to
obtain results as shown in Table 1.
Furthermore, the scattering of the magnetic properties in longitudinal
direction and widthwise direction was measured to obtain results as shown
in FIGS. 8 and 9.
TABLE 1(a)
__________________________________________________________________________
Holding time at
1000-850.degree. C. when
Temperature after
First pass of rolling under
Slab final pass of
finish rolling conditions according
Magnetic properties
No. composition
rough rolling (.degree.C.)
temperature (.degree.C.)
draft (%)
to the invention
B.sub.8 (T)
W.sub.17/50
Remarks
__________________________________________________________________________
1 A 1225 948 57 4 1.922
0.823 acceptable
example
2 A 1251 935 52 7 1.921
0.829 acceptable
example
3 A 1208 967 44 4 1.925
0.825 acceptable
example
4 A 1238 913 56 7 1.924
0.824 acceptable
example
5 A 1202 943 64 5 1.911
0.834 acceptable
example
6 B 1247 903 45 4 1.920
0.830 acceptable
example
7 B 1173 889 43 3 1.918
0.831 acceptable
example
8 B 1214 923 51 5 1.932
0.822 acceptable
example
9 B 1178 932 48 6 1.925
0.827 acceptable
example
10 A 1145* 903 57 3 1.891
0.867 comparative
example
11 A 1139* 910 48 5 1.880
0.891 comparative
example
12 B 1120* 861 49 4 1.883
0.903 comparative
example
__________________________________________________________________________
TABLE 1(b)
__________________________________________________________________________
Holding time at
1000-850.degree. C. when
Temperature after
First pass of rolling under
Slab final pass of
finish rolling conditions according
Magnetic properties
No. composition
rough rolling (.degree.C.)
temperature (.degree.C.)
draft (%)
to the invention
B.sub.8 (T)
W.sub.17/50
Remarks
__________________________________________________________________________
13 A 1217 908 35* 5 1.892
0.892 comparative
example
14 A 1178 895 30* 5 1.887
0.903 comparative
example
15 B 1221 881 33* 3 1.882
0.901 comparative
example
16 A 1164 841* 41 -- 1.860
0.912 comparative
example
17 B 1162 832* 50 -- 1.872
0.917 comparative
example
18 A 1218 946 45 21* 1.860
0.903 comparative
example
19 B 1160 863 42 1.5* 1.887
0.891 comparative
example
20 A 1145* 845* 38* -- 1.878
0.918 comparative
example
21 A 1166 856 38* 1.5* 1.873
0.906 comparative
example
22 A 1205 972 45 3 1.910
0.823 acceptable
example
23 B 1231 968 63 4 1.915
0.824 acceptable
example
24 A 1232 995 43 21* 1.871
0.909 comparative
example
__________________________________________________________________________
*outside scope of the invention
As seen from Table 1 and FIGS. 8 and 9, when the first pass in the finish
rolling is carried out at a temperature of 1000.degree.-850.degree. C. and
a draft of not less than 40% and this temperature is held for 2-20
seconds, not only the magnetic properties are excellent, but also the
uniformity of the magnetic properties in the widthwise direction and
longitudinal direction is excellent.
EXAMPLE 2
(C) Continuously cast slab comprising C: 0.040%, Si: 3.14%, Mn: 0.054%, Se:
0.023%, Sb: 0.024%, Mo: 0.020% and the remainder being substantially Fe.
(D) Continuously cast slab comprising C: 0.039%, Si: 3.30%, Mn: 0.054%, Se:
0.019%, Sn: 0.082% and the remainder being substantially Fe.
(E) Continuously cast slab comprising C: 0.040%, Si: 3.30%, Mn: 0.054%, Se:
0.022%, Sb: 0.024%, As: 0.020% and the remainder being substantially Fe.
(F) Continuously cast slab comprising C: 0.040%, Si: 3.30%, Mn: 0.054%, Se:
0.022%, Sb: 0.024%, Cu: 0.04% and the remainder being substantially Fe.
(G) Continuously cast slab comprising C: 0.040%, Si: 3.30%, Mn: 0.054%, Se:
0.022%, Sb: 0.024%, Bi: 0.02% and the remainder being substantially Fe.
(H) Continuously cast slab comprising C: 0.040%, Si: 3.30%, Mn: 0.054%, Se:
0.022% and the remainder being substantially Fe.
(I) Continuously cast slab comprising C: 0.036%, Si: 3.01%, Mn: 0.069%, Se:
0.023%, Sb: 0.020%, Al: 0.021%, N: 0.008% and the remainder being
substantially Fe.
Each of the above slabs was placed in a heating furnace, soaked in an
N.sub.2 atmosphere, and then subjected to a rough rolling just after the
soaking. The rough rolling was carried out through 5-6 passes in
accordance with the slab thickness under such a condition that the draft
at each pass was approximately equal, whereby a sheet bar of 30 mm in
thickness was obtained. Then, the sheet bar was hot rolled in a tandem
mill to obtain a hot rolled steel sheet of 2.0 mm in thickness. The
temperature after the final pass of the rough rolling and conditions in
first pass of the finish rolling are shown in Table 2.
The hot rolled steel sheet was pickled, subjected to first cold rolling and
intermediate annealing and further to second cold rolling to obtain a cold
rolled steel sheet having a final thickness of 0.23 mm. Thereafter, the
cold rolled steel sheet was subjected to decarburization annealing, coated
with a slurry of an annealing separator consisting mainly of MgO, and then
subjected to a final finish annealing comprised of secondary
recrystallization annealing and purification annealing to obtain a
product.
The magnetic properties of the thus obtained product were measured to
obtain results as shown in Table 2. In any slab compositions, the products
obtained according to the invention are excellent as compared with the
comparative examples.
TABLE 2
__________________________________________________________________________
Holding time at
1000-850.degree. C. when
Temperature after
First pass of rolling under
Slab final pass of
finish rolling conditions according
Magnetic properties
No. composition
rough rolling (.degree.C.)
temperature (.degree.C.)
draft (%)
to the invention
B.sub.8 (T)
W.sub.17/50
Remarks
__________________________________________________________________________
25 C 1235 948 54 4 1.921
0.832 acceptable
example
26 C 1251 835* 52 1.4* 1.891
0.899 comparative
example
27 D 1208 867 46 4 1.924
0.823 acceptable
example
28 D 1113* 903 53 6 1.884
0.901 comparative
example
29 E 1202 943 63 5 1.913
0.835 acceptable
example
30 E 1247 903 38* 4 1.899
0.911 comparative
example
31 F 1173 889 45 3 1.917
0.832 acceptable
example
32 F 1250 923 43 21* 1.882
0.921 comparative
example
33 G 1178 932 48 6 1.924
0.826 acceptable
example
34 G 1145* 903 57 3 1.901
0.877 comparative
example
35 H 1253 940 55 3 1.922
0.830 acceptable
example
36 H 1246 910 35* 5 1.882
0.920 comparative
example
37 I 1252 938 60 4 1.923
0.832 acceptable
example
38 I 1220 840* 57 3 1.901
0.930 comparative
example
__________________________________________________________________________
*outside scope of the invention
EXAMPLE 3
(J) Continuously cast slab comprising C: 0.040%, Si: 3.14%, Mn: 0.054%, Se:
0.023%, Sb: 0.024%, Al: 0.022%, N: 0.008%, Mo: 0.020% and the remainder
being substantially Fe.
(K) Continuously cast slab comprising C: 0.039%, Si: 3.30%, Mn: 0.054%, Se:
0.019%, Sb: 0.022%, Al: 0.023%, N: 0.008%, Sn: 0.080% and the remainder
being substantially Fe.
(L) Continuously cast slab comprising C: 0.039%, Si: 3.29%, Mn: 0.053%, Se:
0.020%, Sb: 0.023%, Al: 0.020%, N: 0.009%, As: 0.020% and the remainder
being substantially Fe.
(M) Continuously cast slab comprising C: 0.040%, Si: 3.29%, Mn: 0.054%, Se:
0.021%, Sb: 0.024%, Al: 0.022%, N: 0.008%, Cu: 0.04% and the remainder
being substantially Fe.
(N) Continuously cast slab comprising C: 0.038%, Si: 3.31%, Mn: 0.054%, Se:
0.022%, Sb: 0.024%, Al: 0.024%, N: 0.008%, Bi: 0.02% and the remainder
being substantially Fe.
Each of the above slabs was placed in a heating furnace, soaked in an
N.sub.2 atmosphere, and then subjected to a rough rolling just after the
soaking. The rough rolling was carried out through 5-6 passes in
accordance with the slab thickness under such a condition that the draft
at each pass was approximately equal, whereby a sheet bar of 30 mm in
thickness was obtained. Then, the sheet bar was hot rolled in a tandem
mill to obtain a hot rolled steel sheet of 2.0 mm in thickness. The
temperature after the final pass of the rough rolling and conditions in
first pass of the finish rolling are shown in Table 3.
The hot rolled steel sheet was pickled, subjected to first cold rolling and
intermediate annealing and further to second cold rolling to obtain a cold
rolled steel sheet having a final thickness of 0.23 mm. Thereafter, the
cold rolled steel sheet was subjected to decarburization annealing, coated
with a slurry of an annealing separator consisting mainly of MgO, and then
subjected to a final finish annealing comprised of secondary
recrystallization annealing and purification annealing to obtain a
product.
The magnetic properties of the thus obtained product were measured to
obtain results as shown in Table 3. In any slab compositions, the products
obtained according to the invention are excellent as compared with the
comparative examples.
TABLE 3
__________________________________________________________________________
Holding time at
1000-850.degree. C. when
Temperature after
First pass of rolling under
Slab final pass of
finish rolling conditions according
Magnetic properties
No. composition
rough rolling (.degree.C.)
temperature (.degree.C.)
draft (%)
to the invention
B.sub.8 (T)
W.sub.17/50
Remarks
__________________________________________________________________________
39 J 1245 947 54 4 1.924
0.822 acceptable
example
40 J 1241 834* 50 1.6* 1.891
0.903 comparative
example
41 K 1232 891 50 4 1.921
0.820 acceptable
example
42 K 1115* 920 48 4 1.880
0.899 comparative
example
43 L 1230 949 53 5 1.919
0.822 acceptable
example
44 L 1245 910 35* 4 1.890
0.901 comparative
example
45 M 1210 912 51 3 1.918
0.830 acceptable
example
46 M 1242 948 43 21* 1.883
0.926 comparative
example
47 N 1192 939 52 5 1.922
0.825 acceptable
example
48 N 1145* 903 57 3 1.899
0.897 comparative
example
__________________________________________________________________________
*outside scope of the invention
EXAMPLE 4
(O) Continuously cast slab comprising C: 0.041%, Si: 3.10%, Mn: 0.074%, Se:
0.021% and the remainder being substantially Fe.
(P) Continuously cast slab comprising C: 0.040%, Si: 3.29%, Mn: 0.064%, Se:
0.020%, Sb: 0.024% and the remainder being substantially Fe.
(Q) Continuously cast slab comprising C: 0.035%, Si: 3.00%, Mn: 0.072%, Se:
0.023%, Al: 0.023%, N: 0.008% and the remainder being substantially Fe.
Each of the above slabs was immediately placed in a gas heating furnace,
soaked in an N.sub.2 atmosphere, further placed into an induction heating
furnace, at where a temperature difference between temperature of central
portion being 1430.degree. C. and temperature of surface portion being
1370.degree. C. was sufficiently ensured, and immediately subjected to a
rough rolling. The rough rolling was carried out through 5-6 passes in
accordance with the slab thickness under such a condition that the draft
at each pass was approximately equal, whereby a sheet bar of 40 mm in
thickness was obtained. Moreover, the surface was positively cooled during
the rough rolling. Then, the sheet bar was hot rolled in a tandem mill to
obtain a hot rolled steel sheet of 3.0 mm in thickness. In this case, the
surface of the sheet bar was sufficiently cooled with a high pressure
water prior to the finish rolling. The conditions of the finish rolling
are shown in Table 4.
The hot rolled steel sheet was pickled, subjected to first cold rolling and
intermediate annealing and further to second cold rolling to obtain a cold
rolled steel sheet having a final thickness of 0.23 mm. Thereafter, the
cold rolled steel sheet was subjected to decarburization annealing, coated
with a slurry of an annealing separator consisting mainly of MgO, and then
subjected to a final finish annealing comprised of secondary
recrystallization annealing and purification annealing to obtain a
product.
The magnetic properties of the thus obtained product were measured to
obtain results as shown in Table 4.
TABLE 4(a)
__________________________________________________________________________
First pass of finish rolling
At central
Use temperature temperature
Slab method of
of central
in 1/20 layer
of 950-850.degree. C.
composi-
heating
draft
portion
temperature
holding
draft
holding
Magnetic properties
No.
tion furnace
(%)
(.degree.C.)
(.degree.C.)
time (s)
(%)
time (s)
B.sub.8 (T)
W.sub.17/50
Remarks
__________________________________________________________________________
49 O .largecircle.
42 1151 970 4 45 3 1.922
0.970 acceptable
example
50 O .DELTA.
50 1153 995 5 43 4 1.925
0.968 acceptable
example
51 O .largecircle.
43 1155 990 7 56 3 1.912
0.972 acceptable
example
52 O .DELTA.
46 1160 996 6 60 5 1.911
0.971 acceptable
example
53 O .largecircle.
47 1154 965 5 51 6 1.919
0.978 acceptable
example
54 O .largecircle.
48 1110* 960 3 45 7 1.890
1.051 comparative
example
55 O .DELTA.
38*
1153 970 4 35*
2 1.900
1.020 comparative
example
56 O .largecircle.
45 1163 981 4 42 1* 1.883
1.031 comparative
example
57 O .largecircle.
43 1160 1030* -- 54 4 1.882
1.003 comparative
example
58 O X 48 1145* 1050* -- 53 5 1.872
1.041 comparative
example
59 P .largecircle.
46 1160 973 5 48 5 1.930
0.969 acceptable
example
60 P .DELTA.
52 1172 980 4 55 5 1.910
0.970 acceptable
example
61 P .largecircle.
53 1159 990 3 65 4 1.913
0.980 acceptable
example
__________________________________________________________________________
TABLE 4(b)
__________________________________________________________________________
First pass of finish rolling
At central
Use temperature temperature
Slab method of
of central
in 1/20 layer
of 950-850.degree. C.
composi-
heating
draft
portion
temperature
holding
draft
holding
Magnetic properties
No.
tion furnace
(%)
(.degree.C.)
(.degree.C.)
time (s)
(%)
time (s)
B.sub.8 (T)
W.sub.17/50
Remarks
__________________________________________________________________________
62 P .largecircle.
45 1131* 975 2 70 3 1.821
1.035 comparative
example
63 P .largecircle.
48 1162 1060* -- 63 2 1.830
1.050 comparative
example
64 P .largecircle.
49 1160 953 1* 54 3 1.822
1.052 comparative
example
65 P .DELTA.
45 1163 965 5 30*
3 1.873
1.041 comparative
example
66 P .largecircle.
45 1168 983 3 66 1* 1.881
1.054 comparative
example
67 P X 62 1105* 998 5 55 3 1.889
1.053 comparative
example
68 Q .DELTA.
51 1173 973 6 45 4 1.925
0.965 acceptable
example
69 Q .largecircle.
49 1172 965 4 63 3 1.919
0.975 acceptable
example
70 Q .largecircle.
53 1164 969 3 35*
2 1.891
1.057 comparative
example
71 Q .largecircle.
49 1153 976 1* 56 3 1.870
1.063 comparative
example
72 Q X 52 1020* 945* -- 71 5 1.873
1.055 comparative
example
73 Q .largecircle.
53 1180 1006* -- 54 3 1.885
1.049 comparative
example
74 Q X 35*
1082 997 6 46 4 1.860
1.056 comparative
example
__________________________________________________________________________
Note 1: Use method of heating furnace
.largecircle.: gas furnace + induction heating furnace
.DELTA.: only induction heating furnace
X: only gas furnace
Note 2: outside scope of the invention
As seen from Table 4, when the first pass of the finish rolling is carried
out under conditions that the draft is not less than 40% at the
temperature of the 1/20 layer of 1000.degree. C.-950.degree. C. and this
temperature is held for 3-20 seconds and further the working strain at a
draft of not less than 40% is applied at the temperature of the central
portion of 950.degree. C.-850.degree. C. and this temperature is held for
2-20 seconds, the improved magnetic properties are stably obtained.
In Table 4 is also shown a case using no induction heating furnace. In this
case, it is very difficult to take the temperature difference and the
temperature difference between the surface layer and the central portion
hardly ensures, so that the properties are not stably obtained.
EXAMPLE 5
A continuously cast slab comprising C: 0.043%, Si: 3.08%, Mn: 0.070%, Se:
0.022%, Sb: 0.020% and the remainder being substantially Fe was
immediately placed in a gas heating furnace, soaked in an N.sub.2
atmosphere to render the temperature of central portion into 1370.degree.
C. and the temperature of surface portion into 1410.degree. C., and
immediately subjected to a rough rolling. The rough rolling was carried
out through 5-6 passes in accordance with the slab thickness under such a
condition that the draft at each pass was approximately equal, whereby a
sheet bar of 30 mm in thickness was obtained. Then, the sheet bar was hot
rolled in a tandem mill to obtain a hot rolled steel sheet of 2.0 mm in
thickness. The conditions of the finish rolling are shown in Table 5.
On the other hand, each continuously cast slab having the above composition
was immediately placed in a gas heating furnace, soaked in an N.sub.2
atmosphere, further placed into an induction heating furnace, where the
temperature difference between the temperature of the central portion at
1430.degree. C. and the temperature of the surface portion at 1370.degree.
C. was sufficiently ensured, and immediately subjected to a rough rolling.
The rough rolling was carried out under the same conditions as described
above, whereby a sheet bar of 40 mm in thickness was obtained. Moreover,
the surface was positively cooled during the rough rolling. Then, the
sheet bar was hot rolled in a tandem mill to obtain a hot rolled steel
sheet of 2.0 mm in thickness. The conditions of the finish rolling are
shown in Table 5.
The hot rolled steel sheet was pickled, subjected to first cold rolling and
intermediate annealing and further to second cold rolling to obtain a cold
rolled steel sheet having a final thickness of 0.23 mm. Thereafter, the
cold rolled steel sheet was subjected to decarburization annealing, coated
with a slurry of an annealing separator consisting mainly of MgO, and then
subjected to a final finish annealing comprised of secondary
recrystallization annealing and purification annealing to obtain a
product.
The magnetic properties of the thus obtained product were measured to
obtain results as shown in Table 5.
In Table 5 are also shown results measured on a case that the temperature
of the decarburization annealing at the above steps is shifted to
20.degree. C. higher than the optimum temperature.
From this table, it is understood that when the inhibitor in the hot rolled
sheet is controlled at the direction of sheet thickness, the magnetic
properties can stably be improved even in the change of treating
conditions frequently generated in the actual running line.
TABLE 5
__________________________________________________________________________
Ratio of achieving
B.sub.8
of not more than 190
T
First pass of finish rolling
At central temperature when decarburization
temperature of in 1/20 layer
of 950-850.degree. C. annealing is carried
draft
central portion
temperature
holding
draft
holding
Magnetic properties
out at a temperature
No.
(%)
(.degree.C.)
(.degree.C.)
time (s)
(%) time (s)
B.sub.8 (T)
W.sub.17/50 (W/kg)
higher by 20.degree.
__________________________________________________________________________
C.
1 55 1155 970 5 51 4 1.923
0.830 10
2 48 1151 995 4 49 3 1.925
0.835 8
3 57 1154 991 7 52 5 1.915
0.829 11
4 56 1000 996 6 -- -- 1.911
0.839 50
5 51 995 965 5 -- -- 1.909
0.826 65
6 48 989 960 3 -- -- 1.915
0.839 48
__________________________________________________________________________
EXAMPLE 6
A continuously cast slab comprising C: 0.040%, Si: 3.30%, Mn: 0.054%, Se:
0.022%, Sb: 0.024% and the remainder being substantially Fe was placed
into a heating furnace, soaked in an N.sub.2 atmosphere, and subjected to
a rough rolling under conditions as shown in Table 6 immediately after the
soaking, whereby a sheet bar of 30 mm in thickness was obtained.
Then, the sheet bar was hot rolled in a tandem mill to obtain a hot rolled
steel sheet of 2.0 mm in thickness. The hot rolled steel sheet was pickled
and subjected to first cold rolling--intermediate annealing --second cold
rolling to obtain a cold rolled steel sheet having a final thickness of
0.23 mm. Thereafter, the sheet was subjected to decarburization annealing,
coated with a slurry of an annealing separator consisting mainly of MgO,
and subjected to a final finish annealing comprised of secondary
recrystallization annealing and purification annealing to obtain a
product.
The magnetic properties, surface properties and ratio of poor secondary
recrystallized portion in the widthwise direction of the thus obtained
product were measured to obtain results shown in Table 6.
Furthermore, results measured on the scattering of magnetic flux density in
the longitudinal direction of the steel sheet are shown in FIG. 10.
TABLE 6(a)
__________________________________________________________________________
Ratio of
Final pass of abnormal
Slab First pass of rough rolling
rough rolling
Magnetic
Ratio of
grains in
heating temper- interval time
temper- properties
spill widthwise
temper-
ature T.sub.1
draft R.sub.1
between passes
ature T.sub.2
draft R.sub.2
B.sub.8
W.sub.17/50
generated
direction
No.
ature (.degree.C.)
(.degree.C.)
(%) (s) (.degree.C.)
(%) (T)
(W/kg)
(%) (%) Remarks
__________________________________________________________________________
1 1435 1363 59 43 1228 47 1.922
0.822
0.30 0.12 acceptable
example
2 1433 1348 36 110 1215 53 1.923
0.833
0.24 0.21 acceptable
example
3 1442 1330 31 71 1208 59 1.921
0.831
0.24 0.18 acceptable
example
4 1421 1352 51 64 1248 59 1.924
0.830
0.27 0.17 acceptable
example
5 1385 1311 56 36 1228 60 1.925
0.825
0.31 0.14 acceptable
example
6 1423 1341 48 45 1249 45 1.920
0.837
0.22 0.20 acceptable
example
7 1390 1328 39 59 1202 46 1.923
0.828
0.26 0.23 acceptable
example
8 1410 1337 20 95 1245 67 1.927
0.815
0.24 0.19 acceptable
example
9 1395 1305 24 75 1209 68 1.934
0.819
0.29 0.24 acceptable
example
__________________________________________________________________________
TABLE 6(b)
__________________________________________________________________________
Ratio of
Final pass of abnormal
Slab First pass of rough rolling
rough rolling
Magnetic
Ratio of
grains in
heating temper- interval time
temper- properties
spill widthwise
temper-
ature T.sub.1
draft R.sub.1
between passes
ature T.sub.2
draft R.sub.2
B.sub.8
W.sub.17/50
generated
direction
No.
ature (.degree.C.)
(.degree.C.)
(%) (s) (.degree.C.)
(%) (T)
(W/kg)
(%) (%) Remarks
__________________________________________________________________________
10 1405 1302 42 55 1237 50 1.926
0.834
0.27 0.27 acceptable
example
11 1375 1283 31 78 1266 53 1.931
0.827
0.31 0.25 acceptable
example
12 1380 1281 58 50 1251 45 1.928
0.828
0.19 0.28 acceptable
example
13 1440 1323 44 24* 1210 47 1.904
0.851
0.45 3.24 compar-
ative
example
14 1370 1285 63* 32 1140*
55 1.903
0.897
1.67 2.24 compar-
ative
example
15 1365 1196*
58* 25* 1134*
28* 1.897
0.906
1.77 2.77 compar-
ative
example
16 1388 1246*
24* 35 1267 40 1.886
0.943
3.27 3.15 compar-
ative
example
17 1366 1185*
42* 33 1084*
30* 1.891
0.913
2.24 4.26 compar-
ative
example
18 1408 1291 33 26* 1208 50 1.892
0.905
2.68 3.42 compar-
ative
example
__________________________________________________________________________
*outside scope of the invention
As seen from Table 6 and FIG. 10, when the rough rolling is carried out at
a high temperature and a large draft according to the invention, the
secondary recrystallization uniformly proceeds in the widthwise direction
to provide improved magnetic properties, and also the surface properties
are good and further the uniformity of the magnetic properties in the
longitudinal direction is excellent.
EXAMPLE 7
A continuously cast slab comprising C: 0.035%, Si: 2.98%, Mn: 0.072%, S:
0.018% and the remainder being substantially Fe was placed into a heating
furnace, soaked in an N.sub.2 atmosphere, and subjected to a rough rolling
under conditions as shown in Table 7 immediately after the soaking,
whereby a sheet bar of 35 mm in thickness was obtained.
Then, the sheet bar was hot rolled in a tandem mill to obtain a hot rolled
steel sheet of 2.4 mm in thickness. The hot rolled steel sheet was pickled
and subjected to first cold rolling--intermediate annealing --second cold
rolling to obtain a cold rolled steel sheet having a final thickness of
0.35 mm. Thereafter, the sheet was subjected to decarburization annealing,
coated with a slurry of an annealing separator consisting mainly of MgO,
and subjected to a final finish annealing comprised of secondary
recrystallization annealing and purification annealing to obtain a
product.
The magnetic properties, surface properties and ratio of poor secondary
recrystallized portion in widthwise direction of the thus obtained product
were measured to obtain results shown in Table 7.
TABLE 7
__________________________________________________________________________
Ratio of
Final pass of abnormal
Slab First pass of rough rolling
rough rolling
Magnetic
Ratio of
grains in
heating temper- interval time
temper- properties
spill widthwise
temper-
ature T.sub.1
draft R.sub.1
between passes
ature T.sub.2
draft R.sub.2
B.sub.8
W.sub.17/50
generated
direction
No.
ature (.degree.C.)
(.degree.C.)
(%) (s) (.degree.C.)
(%) (T)
(W/kg)
(%) (%) Remarks
__________________________________________________________________________
1 1437 1343 52 31 1232 44 1.882
1.263
0.42 0.11 acceptable
example
2 1381 1285 45 44 1208 55 1.879
1.271
0.38 0.22 acceptable
example
3 1408 1283 40 14* 1182*
47 1.856
1.407
1.15 3.54 compar-
ative
example
4 1367 1242*
53 63 1234 45 1.849
1.418
1.54 2.79 compar-
ative
example
__________________________________________________________________________
*outside scope of the invention
As seen from Table 7, when the rough rolling is carried out at a high
temperature and a large draft according to the invention, the secondary
recrystallization uniformly proceeds in the widthwise direction to provide
improved magnetic properties, and also the surface properties are good and
further the uniformity of the magnetic properties in the longitudinal
direction is excellent.
EXAMPLE 8
A continuously cast slab comprising C: 0.050%, Si: 3.10%, Mn: 0.078%, S:
0.024%, Al: 0.032%, N: 0.006% and the remainder being substantially Fe was
placed into a heating furnace, soaked in an N.sub.2 atmosphere, and
subjected to a rough rolling under conditions as shown in Table 6
immediately after the soaking, whereby a sheet bar of 30 mm in thickness
was obtained.
Then, the sheet bar was hot rolled in a tandem mill to obtain a hot rolled
steel sheet of 2.3 mm in thickness. The hot rolled steel sheet was pickled
and subjected to first cold rolling--intermediate annealing --second cold
rolling to obtain a cold rolled steel sheet having a final thickness of
0.23 mm. Thereafter, the sheet was subjected to decarburization annealing,
coated with a slurry of an annealing separator consisting mainly of MgO,
and subjected to a final finish annealing comprised of secondary
recrystallization annealing and purification annealing to obtain a
product.
The magnetic properties, surface properties and ratio of poor secondary
recrystallized portion in widthwise direction of the thus obtained product
were measured to obtain results shown in Table 8.
TABLE 8
__________________________________________________________________________
Ratio of
Final pass of abnormal
Slab First pass of rough rolling
rough rolling
Magnetic
Ratio of
grains in
heating temper- interval time
temper- properties
spill widthwise
temper-
ature T.sub.1
draft R.sub.1
between passes
ature T.sub.2
draft R.sub.2
B.sub.8
W.sub.17/50
generated
direction
No.
ature (.degree.C.)
(.degree.C.)
(%) (s) (.degree.C.)
(%) (T)
(W/kg)
(%) (%) Remarks
__________________________________________________________________________
1 1431 1344 23 37 1242 41 1.934
0.861
0.21 0.21 acceptable
example
2 1421 1283 47 69 1218 57 1.938
0.864
0.41 0.25 acceptable
example
3 1401 1293 41 14* 1168*
32* 1.914
0.903
1.21 3.72 compar-
ative
example
4 1366 1244*
54 51 1214 46 1.909
0.899
1.74 2.34 compar-
ative
example
__________________________________________________________________________
*outside scope of the invention
As seen from Table 8, when the rough rolling is carried out at a high
temperature and a large draft according to the invention, the secondary
recrystallization uniformly proceeds in the widthwise direction to provide
improved magnetic properties, and also the surface properties are good and
further the uniformity of the magnetic properties in the longitudinal
direction is excellent.
EXAMPLE 9
(a) Continuously cast slab comprising C: 0.042%, Si: 3.34%, Mn: 0.062%, Se:
0.021%, Sb: 0.025% and the remainder being substantially Fe.
(b) Continuously cast slab comprising C: 0.052%, Si: 3.04%, Mn: 0.070%, Se:
0.023%, Al: 0.025%, N: 0.0077% and the remainder being substantially Fe.
Each of the above slabs was placed in a heating furnace, soaked in an
N.sub.2 atmosphere, and immediately subjected to a rough rolling to obtain
a sheet bar of 30 mm in thickness, which was hot rolled in a tandem mill
to obtain a hot rolled steel sheet of 2.0 mm in thickness. The rough
rolling conditions and conditions of first pass in the finish rolling are
shown in Table 9.
The hot rolled steel sheet was pickled and subjected to first cold rolling
and intermediate annealing and further to second cold rolling to obtain a
cold rolled steel sheet having a final thickness of 0.23 mm. The sheet was
subjected to decarburization annealing, coated with a slurry of an
annealing separator consisting mainly of MgO, and subjected to final
finish annealing comprised of secondary recrystallization annealing and
purification annealing to obtain a product.
The magnetic properties, surface properties and ratio of poor secondary
recrystallized portion in widthwise direction of the thus obtained product
were measured to obtain results shown in Table 9.
TABLE 9(a)
__________________________________________________________________________
First pass of rough rolling
Final pass of rough rolling
First pass of
Slab heating
temper- interval time
temper- final finish rolling
Slab temperature
ature T.sub.1
draft R.sub.1
between passes
ature T.sub.2
draft R.sub.2
temperature
draft
temperature
No. composition
(.degree.C.)
(.degree.C.)
(%) (s) (.degree.C.)
(%) (.degree.C.)
(%)
(.degree.C.)
__________________________________________________________________________
1 a 1435 1363 59 43 1228 47 1225 57 948
2 a 1375 1283 31 78 1266 53 1251 52 935
3 a 1433 1348 36 110 1215 53 1208 44 967
4 a 1421 1352 51 64 1248 59 1238 56 913
5 a 1442 1330 31 71 1208 59 1202 64 943
6 a 1395 1305 24 75 1209 68 1205 45 972
7 a 1433 1348 36 110 1215 53 1208 44 967
8 a 1442 1330 31 71 1208 59 1202 64 943
9 a 1421 1352 51 64 1248 59 1238 56 913
10 a 1385 1311 56 36 1228 60 1225 57 948
11 a 1423 1341 48 45 1249 45 1238 56 913
12 a 1390 1328 39 59 1202 46 1200 45 972
13 a 1410 1337 20 95 1245 67 1238 56 913
__________________________________________________________________________
TABLE 9(b)
__________________________________________________________________________
Holding time at 1000- 850.degree. C. Ratio of abnormal
when rolling under conditions
Magnetic properties
Ratio of spill
grains in widthwise
No. according to the invention
B.sub.8 (T)
W.sub.17/50 (W/kg)
generated (%)
direction (%)
Remarks
__________________________________________________________________________
1 4 1.927
0.818 0.30 0.12 acceptable example
2 7 1.926
0.824 0.31 0.25 acceptable example
3 4 1.929
0.820 0.24 0.21 acceptable example
4 7 1.929
0.819 0.27 0.17 acceptable example
5 5 1.926
0.828 0.24 0.18 acceptable example
6 3 1.936
0.818 0.29 0.24 acceptable example
7 4 1.928
0.828 0.24 0.21 acceptable example
8 5 1.926
0.826 0.24 0.18 acceptable example
9 7 1.929
0.825 0.27 0.17 acceptable example
10 4 1.930
0.821 0.31 0.14 acceptable example
11 7 1.926
0.829 0.22 0.20 acceptable example
12 3 1.928
0.822 0.26 0.23 acceptable example
13 7 1.937
0.811 0.24 0.19 acceptable
__________________________________________________________________________
example
TABLE 9(c)
__________________________________________________________________________
First pass of rough rolling
Final pass of rough rolling
First pass of
Slab heating
temper- interval time
temper- final finish rolling
Slab temperature
ature T.sub.1
draft R.sub.1
between passes
ature T.sub.2
draft R.sub.2
temperature
draft
temperature
No. composition
(.degree.C.)
(.degree.C.)
(%) (s) (.degree.C.)
(%) (.degree.C.)
(%)
(.degree.C.)
__________________________________________________________________________
14 a 1395 1305 24 75 1209 68 1205 45 972
15 a 1405 1302 42 55 1237 50 1225 57 948
16 a 1375 1283 31 78 1266 53 1251 52 935
17 a 1380 1281 58 50 1251 45 1238 56 913
18 a 1388 1246*
24* 35 1167*
40 1151* 52 935
19 a 1370 1285 63* 32 1140*
55 1139* 48 910
20 a 1365 1196*
58* 25* 1134*
28* 1111* 38*
845*
21 a 1366 1185*
42*
33 1084*
30* 1066* 38*
856
22 b 1375 1283 31 78 1266 53 1247 45 903
23 b 1395 1305 24 75 1209 68 1173 43 889
24 b 1385 1311 56 36 1228 60 1214 51 923
25 b 1442 1330 31 71 1208 59 1178 48 932
26 b 1423 1341 48 45 1249 45 1231 63 968
27 b 1365 1196*
58* 25* 1134*
28* 1162 50 832*
28 b 1440 1323 44 24* 1210 47 1160 42 863
__________________________________________________________________________
TABLE 9(d)
__________________________________________________________________________
Holding time at 1000- 850.degree. C. Ratio of abnormal
when rolling under conditions
Magnetic properties
Ratio of spill
grains in widthwise
No. according to the invention
B.sub.8 (T)
W.sub.17/50 (W/kg)
generated (%)
direction (%)
Remarks
__________________________________________________________________________
14 3 1.934
0.815 0.29 0.24 acceptable example
15 4 1.929
0.828 0.27 0.27 acceptable example
16 7 1.934
0.822 0.31 0.25 acceptable example
17 7 1.931
0.824 0.19 0.28 acceptable example
18 7 1.886
0.943 3.27 3.15 comparative example
19 5 1.880
0.891 1.67 2.24 comparative example
20 -- 1.878
0.918 1.77 2.77 comparative example
21 1.5* 1.873
0.906 2.24 4.26 comparative example
22 4 1.937
0.821 0.31 0.25 acceptable example
23 3 1.939
0.813 0.29 0.24 acceptable example
24 5 1.936
0.818 0.31 0.14 acceptable example
25 6 1.938
0.821 0.24 0.18 acceptable example
26 4 1.930
0.817 0.22 0.20 acceptable example
27 -- 1.872
0.917 1.77 2.77 comparative example
28 1.5* 1.887
0.891 0.45 3.24 comparative
__________________________________________________________________________
example
*outside scope of the invention
As seen from the above Table, when the rough rolling and the finish rolling
are carried out according to the invention, the magnetic properties and
the surface properties are excellent.
EXAMPLE 10
(c) Continuously cast slab comprising C: 0.041%, Si: 3.18%, Mn: 0.058%, Se:
0.022%, Sb: 0.023%, Mo: 0.020% and the remainder being substantially Fe.
(d) Continuously cast slab comprising C: 0.040%, Si: 3.32%, Mn: 0.056%, Se:
0.020%, Sn: 0.081% and the remainder being substantially Fe.
(e) Continuously cast slab comprising C: 0.041%, Si: 3.33%, Mn: 0.058%, Se:
0.021%, Sb: 0.025%, As: 0.019% and the remainder being substantially Fe.
(f) Continuously cast slab comprising C: 0.042%, Si: 3.28%, Mn: 0.055%, Se:
0.023%, Sb: 0.025%, Cu: 0.05% and the remainder being substantially Fe.
(g) Continuously cast slab comprising C: 0.039%, Si: 3.33%, Mn: 0.059%, Se:
0.021%, Sb: 0.023%, Bi: 0.03% and the remainder being substantially Fe.
(h) Continuously cast slab comprising C: 0.041%, Si: 3.35%, Mn: 0.060%, Se:
0.024% and the remainder being substantially Fe.
(i) Continuously cast slab comprising C: 0.038%, Si: 3.08%, Mn: 0.067%, Se:
0.024%, Sb: 0.024%, Al: 0.022%, N: 0.007% and the remainder being
substantially Fe.
(j) Continuously cast slab comprising C: 0.041%, Si: 3.17%, Mn: 0.059%, Se:
0.022%, Sb: 0.025%, Al: 0.024%, N: 0.007%, Mo: 0.023% and the remainder
being substantially Fe.
(k) Continuously cast slab comprising C: 0.040%, Si: 3.35%, Mn: 0.061%, Se:
0.020%, Sb: 0.023%, Al: 0.021%, N: 0.007%, Sn: 0.084% and the remainder
being substantially Fe.
(l) Continuously cast slab comprising C: 0.041%, Si: 3.34%, Mn: 0.058%, Se:
0.022%, Sb: 0.025%, Al: 0.023%, N: 0.008%, As: 0.023% and the remainder
being substantially Fe.
(m) Continuously cast slab comprising C: 0.039%, Si: 3.35%, Mn: 0.062%, Se:
0.023%, Sb: 0.023%, Al: 0.021%, N: 0.009%, Cu: 0.05% and the remainder
being substantially Fe.
(n) Continuously cast slab comprising C: 0.040%, Si: 3.37%, Mn: 0.052%, Se:
0.020%, Sb: 0.026%, Al: 0.027%, N: 0.007%, Bi: 0.03% and the remainder
being substantially Fe.
Each of the above slabs was placed in a heating furnace, soaked in an
N.sub.2 atmosphere, and immediately subjected to a rough rolling to obtain
a sheet bar of 30 mm in thickness, which was hot rolled in a tandem mill
to obtain a hot rolled steel sheet of 2.0 mm in thickness. The rough
rolling conditions and conditions of first pass in the finish rolling are
shown in Table 10.
The hot rolled steel sheet was pickled and subjected to first cold rolling
and intermediate annealing and further to second cold rolling to obtain a
cold rolled steel sheet having a final thickness of 0.23 mm. The sheet was
subjected to decarburization annealing, coated with a slurry of an
annealing separator consisting mainly of MgO, and subjected to final
finish annealing comprised of secondary recrystallization annealing and
purification annealing to obtain a product.
The magnetic properties, surface properties and ratio of poor secondary
recrystallized portion in widthwise direction of the thus obtained product
were measured to obtain results shown in Table 10. In any slab
compositions, the products obtained according to the invention are
excellent as compared with the comparative examples.
TABLE 10(a)
__________________________________________________________________________
First pass of rough rolling
Final pass of rough rolling
First pass of
Slab heating
temper- interval time
temper- final finish rolling
Slab temperature
ature T.sub.1
draft R.sub.1
between passes
ature T.sub.2
draft R.sub.2
temperature
draft
temperature
No. composition
(.degree.C.)
(.degree.C.)
(%) (s) (.degree.C.)
(%) (.degree.C.)
(%)
(.degree.C.)
__________________________________________________________________________
29 c 1423 1341 48 45 1249 45 1235 54 948
30 c 1395 1305 24 75 1209 68 1208 46 867
31 c 1440 1323 44 24* 1210 47 1208 45 866
32 d 1433 1348 36 110 1215 53 1208 46 867
33 d 1395 1305 24 75 1209 68 1174 46 890
34 d 1388 1246*
24* 35 1167 40 1146* 58 904
35 e 1433 1348 36 110 1215 53 1202 63 943
36 e 1390 1328 39 59 1202 46 1179 49 933
37 e 1365 1196*
58* 25* 1134*
28* 1114* 38*
904
38 f 1385 1311 56 36 1228 60 1173 45 889
39 f 1435 1363 59 43 1228 47 1209 47 868
40 f 1388 1246*
24* 35 1167 40 1146* 58 904
41 g 1405 1302 42 55 1237 50 1178 48 932
42 g 1395 1305 24 75 1209 68 1203 64 944
43 g 1408 1291 33 26* 1208 50 1145* 46 890
44 h 1421 1352 51 64 1258 59 1253 55 940
45 h 1405 1302 42 55 1237 50 1231 54 950
46 h 1370 1285 63* 32 1140*
32 1116* 35*
920
__________________________________________________________________________
TABLE 10(b)
__________________________________________________________________________
Holding time at 1000- 850.degree. C. Ratio of abnormal
when rolling under conditions
Magnetic properties
Ratio of spill
grains in widthwise
No. according to the invention
B.sub.8 (T)
W.sub.17/50 (W/kg)
generated (%)
direction (%)
Remarks
__________________________________________________________________________
29 4 1.927
0.828 0.22 0.20 acceptable example
30 4 1.929
0.819 0.29 0.24 acceptable example
31 1.4* 1.884
0.897 0.45 3.24 comparative example
32 4 1.933
0.813 0.24 0.21 acceptable example
33 3 1.929
0.822 0.29 0.24 acceptable example
34 3 1.886
0.943 3.27 3.15 comparative example
35 5 1.928
0.831 0.24 0.21 acceptable example
36 7 1.926
0.820 0.26 0.23 acceptable example
37 7 1.883
0.900 1.77 2.77 comparative example
38 3 1.925
0.825 0.31 0.14 acceptable example
39 5 1.927
0.822 0.30 0.12 acceptable example
40 21* 1.886
0.878 3.27 3.15 comparative example
41 6 1.929
0.823 0.27 0.27 acceptable example
42 5 1.938
0.816 0.29 0.24 acceptable example
43 4 1.892
0.905 2.68 3.42 comparative example
44 3 1.931
0.825 0.27 0.17 acceptable example
45 6 1.928
0.820 0.28 0.28 acceptable example
46 4 1.880
0.900 1.67 2.24 comparative
__________________________________________________________________________
example
TABLE 10(c)
__________________________________________________________________________
First pass of rough rolling
Final pass of rough rolling
First pass of
Slab heating
temper- interval time
temper- final finish rolling
Slab temperature
ature T.sub.1
draft R.sub.1
between passes
ature T.sub.2
draft R.sub.2
temperature
draft
temperature
No. composition
(.degree.C.)
(.degree.C.)
(%) (s) (.degree.C.)
(%) (.degree.C.)
(%)
(.degree.C.)
__________________________________________________________________________
47 i 1421 1352 51 64 1258 59 1252 60 938
48 i 1385 1311 56 36 1228 60 1177 47 931
49 i 1440 1323 44 24* 1255 47 1250 43 923
50 j 1375 1283 31 78 1266 53 1245 54 947
51 j 1435 1363 59 43 1228 47 1211 52 913
52 j 1440 1323 44 24* 1260 42 1241 50 834*
63 k 1421 1352 51 64 1248 59 1232 50 891
54 k 1385 1311 56 36 1228 60 1172 44 888
55 k 1408 1291 33 26* 1228 50 1222 40 942
56 l 1400 1297 44 53 1237 50 1230 53 949
57 l 1390 1300 44 51 1233 52 1200 63 943
58 l 1410 1293 32 26* 1258 50 1245 35*
910
59 m 1442 1330 31 71 1238 56 1210 51 912
60 m 1423 1341 48 45 1249 45 1230 49 890
61 m 1408 1283 40 14* 1254 45 1244 35*
908
62 n 1410 1337 20 95 1245 67 1192 52 939
63 n 1405 1302 42 55 1237 50 1202 63 943
64 n 1440 1323 44 24* 1255 44 1240 43 948
__________________________________________________________________________
TABLE 10(d)
__________________________________________________________________________
Holding time at 1000- 850.degree. C. Ratio of abnormal
when rolling under conditions
Magentic properties
Ratio of spill
grains in widthwise
No. according to the invention
B.sub.8 (T)
W.sub.17/50 (W/kg)
generated (%)
direction (%)
Remarks
__________________________________________________________________________
47 4 1.939
0.827 0.27 0.17 acceptable example
48 5 1.941
0.823 0.31 0.14 acceptable example
49 12* 1.881
0.920 0.45 3.24 comparative example
50 4 1.938
0.816 0.30 0.24 acceptable example
51 4 1.942
0.820 0.30 0.12 acceptable example
52 1.6* 1.891
0.903 0.50 3.20 comparative example
53 4 1.936
0.816 0.28 0.18 acceptable example
54 3 1.943
0.824 0.26 0.26 acceptable example
55 21* 1.881
0.936 1.77 4.26 comparative example
56 5 1.938
0.818 0.24 0.31 acceptable example
57 6 1.939
0.826 0.26 0.23 acceptable example
58 4 1.885
0.889 2.66 3.44 comparative example
59 3 1.936
0.825 0.22 0.19 acceptable example
60 4 1.939
0.822 0.20 0.22 acceptable example
61 5 1.878
0.941 1.15 3.54 comparative example
62 5 1.941
0.821 0.24 0.19 acceptable example
62 5 1.939
0.820 0.28 0.28 acceptable example
64 21* 1.883
0.926 1.77 3.24 comparative
__________________________________________________________________________
example
*outside scope of the invention
EXAMPLE 11
A continuously cast slab comprising C: 0.034%, Si: 3.01%, Mn: 0.070%, S:
0.017% and the remainder being substantially Fe was placed in a heating
furnace, soaked in an N.sub.2 atmosphere, and subjected to a rough rolling
under conditions shown in Table 11 immediately after the soaking, whereby
a sheet bar of 35 mm in thickness was obtained. Thereafter, the sheet bar
was subjected to a finish tandem rolling under conditions shown in the
same Table 11 to obtain a hot rolled steel sheet of 2.4 mm in thickness.
The hot rolled steel sheet was pickled and subjected to first cold
rolling--intermediate annealing --second cold rolling to obtain a cold
rolled sheet of 0.35 mm in thickness. Then, the sheet was subjected to
decarburization annealing, coated with MgO, and subjected to a final
finish annealing comprised of secondary recrystallization annealing and
purification annealing to obtain a product.
The magnetic properties, surface properties and ratio of poor secondary
recrystallized portion in widthwise direction of the thus obtained product
were measured to obtain results shown in Table 11.
TABLE 11(a)
__________________________________________________________________________
Slab First pass of rough rolling
Final pass of rough rolling
First pass of
heating interval time final finish rolling
temperature
temperature T.sub.1
draft R.sub.1
between passes
temperature T.sub.2
draft R.sub.2
temperature
draft
temperature
No. (.degree.C.)
(.degree.C.)
(%) (s) (.degree.C.)
(%) (.degree.C.)
(%)
(.degree.C.)
__________________________________________________________________________
1 1437 1343 52 31 1232 44 1225 57 948
2 1381 1285 45 44 1208 55 1202 64 943
3 1367 1242* 53 63 1182* 45 1218 45 946
__________________________________________________________________________
TABLE 11(b)
__________________________________________________________________________
Holding time at 1000- 850.degree. C. Ratio of abnormal
when rolling under conditions
Magentic properties
Ratio of spill
grains in widthwise
No. according to the invention
B.sub.8 (T)
W.sub.17/50 (W/kg)
generated (%)
direction (%)
Remarks
__________________________________________________________________________
1 4 1.885
1.259 0.42 0.11 acceptable example
2 5 1.881
1.261 0.38 0.22 acceptable example
3 21* 1.849
1.418 1.54 2.79 comparative
__________________________________________________________________________
example
*outside scope of the invention
As seen from the above Table, when the rough rolling and the finish rolling
are carried out according to the invention, not only the magnetic
properties and surface properties but also the uniformity of the magnetic
properties in the longitudinal direction are excellent.
EXAMPLE 12
(i) Continuously cast slab comprising C: 0.038%, Si: 3.20%, Mn: 0.070%, Se:
0.021% and the remainder being substantially Fe.
(ii) Continuously cast slab comprising C: 0.041%, Si: 3.28%, Mn: 0.065%,
Se: 0.017%, Sb: 0.023% and the remainder being substantially Fe.
(iii) Continuously cast slab comprising C: 0.036%, Si: 3.11%, Mn: 0.071%,
Se: 0.022%, Al: 0.022%, N: 0.008% and the remainder being substantially
Fe.
Each of the above slabs was immediately placed in a gas heating furnace,
soaked in an N.sub.2 atmosphere, further placed into an induction heating
furnace, at where a temperature difference between temperature of central
portion being 1430.degree. C. and temperature of surface portion being
1370.degree. C. was sufficiently ensured, and immediately subjected to a
rough rolling under conditions shown in Table 12, whereby a sheet bar of
30 mm in thickness was obtained. Moreover, the surface was positively
cooled during the rough rolling. Then, the sheet bar was subjected to a
finish tandem rolling under conditions shown in the same Table 12 to
obtain a hot rolled steel sheet of 2.7 mm in thickness. Prior to the
finish rolling, the surface of the sheet bar was sufficiently cooled with
a high pressure water.
The hot rolled steel sheet was pickled, subjected to first cold rolling and
intermediate annealing and further to second cold rolling to obtain a cold
rolled steel sheet having a final thickness of 0.27 mm. Thereafter, the
cold rolled steel sheet was subjected to decarburization annealing, coated
with a slurry of an annealing separator consisting mainly of MgO, and then
subjected to a final finish annealing comprised of secondary
recrystallization annealing and purification annealing to obtain a
product.
The magnetic properties of the thus obtained product were measured to
obtain results as shown in Table 12.
TABLE 12(a)
__________________________________________________________________________
Slab Final pass of
First pass of finish rolling
heating
First pass of rough rolling
rough rolling
temperature
in 1/20 layer
Slab
Use method
temper-
temper-
draft
interval time
temper-
draft of central
temper-
holding
compo-
of heating
ature
ature T.sub.1
R.sub.1
between passes
ature T.sub.2
R.sub.2
draft
portion
ature
time
No. sition
furnace
(.degree.C.)
(.degree.C.)
(%)
(s) (.degree.C.)
(%)
(%)
(.degree.C.)
(.degree.C.)
(s)
__________________________________________________________________________
1 i .largecircle.
1442 1332 31 71 1207 59 43 1154 981 4
2 i .DELTA.
1425 1341 45 45 1249 45 50 1160 995 5
3 i .largecircle.
1415 1338 23 95 1245 66 45 1158 991 6
4 i .DELTA.
1407 1304 41 55 1237 49 46 1160 990 6
5 i .largecircle.
1387 1282 57 50 1254 45 47 1154 972 4
6 i .largecircle.
1366 1196*
58*
25* 1133*
28*
48 1110* 960 3
7 i X 1370 1285 63*
32 1140*
55 45 1003* 963 4
8 ii .largecircle.
1433 1347 36 109 1215 53 46 1162 973 5
9 ii .DELTA.
1442 1330 30 71 1207 58 50 1170 980 4
10 ii .largecircle.
1423 1352 51 64 1249 59 53 1159 990 4
11 ii .DELTA.
1406 1302 41 54 1237 50 49 1172 965 4
12 ii .largecircle.
1411 1338 20 95 1245 67 48 1153 995 5
13 ii .DELTA.
1408 1291 33 26* 1208 50 49 1160 953 1*
14 ii .largecircle.
1410 1196*
58*
25* 1134*
28*
62 1105* 998 5
15 iii .largecircle.
1433 1349 36 110 1215 53 50 1172 973 6
16 iii .DELTA.
1421 1352 50 64 1248 59 50 1168 980 4
17 iii .largecircle.
1390 1328 40 59 1202 46 51 1167 990 3
18 iii .DELTA.
1406 1302 42 55 1237 50 48 1162 980 4
19 iii .largecircle.
1423 1341 48 45 1248 46 49 1159 966 5
20 iii .DELTA.
1388 1246*
25*
35 1267 52 50 1180 1006*
--
21 iii X 1370 1196*
58*
25* 1134*
51 51 1020* 945*
--
__________________________________________________________________________
Use method of heating furnace
.largecircle.: gas furnace + induction heating furnace
.DELTA.: only induction heating furnace
X: only gas furnace
*outside scope of the invention
TABLE 12(b)
__________________________________________________________________________
At central temperature Ratio of spill
Ratio of abnormal
of 950-850.degree. C. Magnetic properties
generated
grains in widthwise
No. cumulative draft (%)
holding time (s)
B.sub.8 (T)
W.sub.17/50 (W/kg)
(%) direction (%)
Remarks
__________________________________________________________________________
1 44 3 1.928
0.895 0.21 0.19 acceptable example
2 43 4 1.930
0.897 0.23 0.19 acceptable example
3 55 3 1.929
0.899 0.24 0.20 acceptable example
4 58 5 1.932
0.891 0.25 0.24 acceptable example
5 52 5 1.931
0.900 0.18 0.28 acceptable example
6 45 7 1.895
1.031 2.24 3.15 comparative example
7 54 4 1.892
1.001 2.60 3.20 comparative example
8 48 5 1.934
0.899 0.27 0.21 acceptable example
9 55 5 1.935
0.893 0.27 0.21 acceptable example
10 65 4 1.933
0.899 0.24 0.20 acceptable example
11 64 3 1.931
0.904 0.20 0.17 acceptable example
12 43 3 1.929
0.903 0.21 0.20 acceptable example
13 54 3 1.872
1.002 2.69 2.98 comparative example
14 55 3 1.870
1.009 2.72 3.03 comparative example
15 45 4 1.939
0.932 0.30 0.21 acceptable example
16 63 3 1.948
0.947 0.24 0.18 acceptable example
17 55 4 1.940
0.921 0.27 0.14 acceptable example
18 65 5 1.948
0.922 0.29 0.20 acceptable example
19 51 5 1.936
0.923 0.31 0.24 acceptable example
20 56 5 1.870
1.110 2.85 3.15 comparative example
21 71 3 1.865
1.120 2.84 2.77 comparative
__________________________________________________________________________
example
As seen from Table 12, when the rough rolling is carried out at a high
temperature and a large draft and then the first pass of the finish
rolling is carried out under such conditions that the draft is not less
than 40% at the temperature of the 1/20 layer of 1000.degree.
C.-950.degree. C. and this temperature is held for 3-20 seconds and
further the working strain at a draft of not less than 40% is applied at
the temperature of the central portion of 950.degree. C.-850.degree. C.
and this temperature is held for 2-20 seconds, the improved magnetic
properties are stably obtained.
In Table 12 is also shown a case using no induction heating furnace. In
this case, it is very difficult to take the temperature difference and the
temperature difference between the surface layer and the central portion
hardly ensures, so that the properties become not stable.
EXAMPLE 13
A continuously cast slab comprising C: 0.043%, Si: 3.41%, Mn: 0.072%, Se:
0.020%, Sb: 0.020% and the remainder being substantially Fe was
immediately placed in a gas heating furnace, soaked in an N.sub.2
atmosphere render the temperature of central portion into 1370.degree. C.
and the temperature of surface layer portion into 1410.degree. C., and
immediately subjected to a rough rolling under conditions shown in Table
13, whereby a sheet bar of 30 mm in thickness was obtained. Then, the
sheet bar was subjected to a finish tandem rolling under conditions shown
in Table 13 to obtain a hot rolled steel sheet of 2.0 mm in thickness.
On the other hand, the continuously cast slab having the above composition
was immediately placed in a gas heating furnace, soaked in an N.sub.2
atmosphere, further placed into an induction heating furnace, at where a
temperature difference between temperature of central portion being
1430.degree. C. and temperature of surface portion being 1370.degree. C.
was sufficiently ensured, and subjected to a rough rolling and finish
rolling under conditions shown in Table 13, whereby a hot rolled steel
sheet of 2.0 mm in thickness was obtained. Moreover, the surface was
positively cooled during the rough rolling.
These hot rolled steel sheets were pickled, subjected to first cold rolling
and intermediate annealing and further to second cold rolling to obtain a
cold rolled steel sheet having a final thickness of 0.23 mm. Thereafter,
the cold rolled steel sheets were subjected to decarburization
diannealing, coated with a slurry of an annealing separator consisting
mainly of MgO, and then subjected to a final finish annealing comprised of
secondary recrystallization annealing and purification annealing to obtain
products.
The magnetic properties of the thus obtained products were measured to
obtain results as shown in Table 13.
In Table 13 are also shown results measured on a case that the temperature
of the decarburization annealing at the above steps is shifted to
20.degree. C. higher than the optimum temperature.
From this table, it is understood that when the inhibitor in the hot rolled
sheet is controlled at the direction of sheet thickness, the magnetic
properties can stably be improved even in the change of treating
conditions frequently generated in the actual running line.
TABLE 13(a)
__________________________________________________________________________
Final pass of
First pass of finish rolling
Slab First pass of rough rolling
rough rolling
temperature
heating temper- interval time
temper- of central
in 1/20 layer
temperature
ature T.sub.1
draft R.sub.1
between passes
ature T.sub.2
draft R.sub.2
draft
portion
temperature
holding time
No. (.degree.C.)
(.degree.C.)
(%) (s) (.degree.C.)
(%) (%)
(.degree.C.)
(.degree.C.)
(s)
__________________________________________________________________________
1 1436 1348 36 110 1215
53 58 1160 983 5
2 1442 1331 30 70 1208
59 48 1155 974 4
3 1432 1341 48 45 1249
45 58 1167 960 7
4 1416 1337 20 75 1245
67 53 1158 970 4
5 1405 1305 24 75 1209
68 60 1159 981 5
6 1424 1340 47 45 1249
45 55 1000 996 6
7 1410 1337 20 95 1245
65 48 989 960 4
8 1377 1196*
58* 25* 1134*
28* 51 995 965 5
9 1380 1246*
24* 35 1267
40 48 950 917 3
__________________________________________________________________________
*outside scope of the invention
TABLE 13(b)
__________________________________________________________________________
Ratio of achieving
B.sub.8
of not more than 1.90
T
when decarburization
At central temperature Ratio of spill
Ratio of abnormal
annealing is carried
of 950-850.degree. C. Magnetic properties
generated
grains in widthwise
out at a temperature
No.
cumulative draft (%)
holding time (s)
B.sub.8 (T)
W.sub.17/50 (W/kg)
(%) direction (%)
higher by 20.degree.
__________________________________________________________________________
C.
1 51 4 1.936
0.813 0.25 0.13 10
2 63 3 1.931
0.820 0.28 0.17 9
3 54 5 1.937
0.824 0.21 0.20 11
4 53 4 1.933
0.819 0.25 0.23 8
5 52 3 1.935
0.819 0.24 0.27 7
6 -- -- 1.926
0.827 0.25 0.25 53
7 -- -- 1.929
0.830 0.27 0.17 61
8 -- -- 1.910
0.910 3.42 3.32 95
9 -- -- 1.908
0.905 2.98 3.55 91
__________________________________________________________________________
INDUSTRIAL APPLICABILITY
According to the invention, grain oriented silicon steel sheets having
improved magnetic properties over a whole of the steel sheet and good
surface properties can stably be produced.
Furthermore, according to the invention, the merits of the hot strip mill
can be utilized at maximum in the production of the grain oriented silicon
steel sheet, so that not only the improvement of the productivity but also
the energy-saving can be achieved.
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